CN102060286B - Energy consumption nano-fluid material and preparation method thereof - Google Patents
Energy consumption nano-fluid material and preparation method thereof Download PDFInfo
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- CN102060286B CN102060286B CN201010541578XA CN201010541578A CN102060286B CN 102060286 B CN102060286 B CN 102060286B CN 201010541578X A CN201010541578X A CN 201010541578XA CN 201010541578 A CN201010541578 A CN 201010541578A CN 102060286 B CN102060286 B CN 102060286B
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Abstract
The invention provides an energy consumption nano-fluid material and a preparation method thereof. The energy consumption nano-fluid material consists of a multi-walled carbon nanotube which is grafted with a functional group, and polar high-surface tension liquid; and liquid overcoming solid-liquid capillary force to enter a nanopore channel is taken as an energy dissipation principle. The preparation method comprises the following steps of: uniformly mixing the multi-walled carbon nanotube and concentrated nitric acid according to a proper ratio, refluxing at a high temperature, washing the oxidized carbon nanotube to be neutral, performing vacuum drying, uniformly mixing with the mixed liquid of toluene and trimethylchlorosilicane according to a proper ratio, refluxing at the high temperature, washing materials to be neutral, performing vacuum drying, and mixing with the polar high-surface tension liquid. The energy consumption nano-fluid material has high energy consumption capacity and low cost, and does not need drive energy provided from the external environment, the energy density of the energy consumption nano-fluid material is greatly higher than that of energy consumption materials such as a magnetorheological material, a viscous material and the like, and devices are simple.
Description
Technical field
The present invention relates to Materials science, is exactly a kind of power consumption nano-fluid material and preparation method thereof specifically.
Background technology
2005, professor Qiao Yu of Univ California-San Diego USA found that the fluid that is mixed with mesoporous material has higher energy dissipation capacity, and the nano-fluid that aerosil, MCM-41, mesoporous carbon particle etc. and water are formed has carried out correlative study.Discover; Because mesoporous material has great specific surface area and porosity; Cause such nano-fluid material that the mechanical energy of external world's input is converted into material admittedly---the liquid interfacial energy; Energy conversion efficiency is about 10J/g, and is more a lot of greatly than power consumption materials such as conventional shape-memory alloy, high molecular polymers.At present, the characteristics of motion of fluid in the nano-scale confined area received extensive concern, and obtained many achievements in research.
Carbon nanotube is the seamless nano level cylinder that is curled and form by certain helicity by the single or multiple lift graphite flake.Characteristics such as little because of its size, that physical strength is high, specific surface area is big, specific conductivity is high, interfacial effect is strong have obtained widespread use at aspects such as flat-panel monitor, One-dimensional Quantum lead, transmitter, ultracapacitor and hydrogen storage materials.
Because carbon nanotube has regular 1-dimention nano passage, thereby fluid is the restrained motion of fluid in carbon nanotube main the concentrating of the domestic restrained motion research of nano-rings.In this respect, people such as G.Hummer utilize computer simulation, have studied the motion conditions of water in SWCN.Research shows, though carbon nanotube itself is a hydrophobic material, water molecules can flow into automatically and through carbon nanotube, behind the Van der Waals force between reduction tube wall and water molecules, water molecules can not get into and pass through carbon nanotube.People such as J.A.Thomasa utilize computingmachine molecular dynamics simulation method, have studied the characteristics of motion such as density, distribution, flow direction of the inside and outside water molecules of carbon nanotube.Research shows that carbon nanotube caliber size is all influential to mass density, distribution and the flow direction of managing inside and outside water molecules.
Computer mould through Chinese scholars fits experiment can be known, though carbon nanotube itself is a hydrophobic material, if do not carry out surface treatment, water molecules can get into automatically and through carbon nanotube, not possess energy dissipation capacity.Also do not have the research of convection cell characteristics of motion in surface-treated carbon nanotube at present both at home and abroad, do not have the research and the application of carbon nanotube power consumption nano-fluid material yet.
Summary of the invention
The object of the present invention is to provide power consumption nano-fluid material of the high surface tension liquid combination of a kind of surface-treated multi-walled carbon nano-tubes and polarity and preparation method thereof.
The objective of the invention is to realize like this:
Described power consumption nano-fluid material is to form like this: length is that nano level multi-walled carbon nano-tubes is at the pipe inside and outside wall; Mouth of pipe grafting trimethyl silane functional group particularly; The high surface tension liquid of the supporting use polarity of the multi-walled carbon nano-tubes of grafting trimethyl silane functional group; The high surface tension liquid of polarity must can not be soaked into the multi-walled carbon nano-tubes after handling each other, adopts the contact angle of the multi-wall carbon nano-tube tube-surface of measurement liquid after processing and the method for roll angle to select the high surface tension liquid of polarity; The multi-walled carbon nano-tubes powder constituent of water or terepthaloyl moietie or USP Kosher and grafting trimethyl silane functional group has the nano-fluid material of energy dissipation capacity.
Described power consumption nano-fluid preparation methods, step is following:
Step 1: with diameter less than 8nm; Purity is 68% the concentrated nitric acid mixed by 1g: 100mL greater than 95% multi-walled carbon nano-tubes and concentration; The normal temperature lower magnetic force stirs 10min; Pour mixed solution into 100 ℃ of oil bath reflux of round-bottomed flask 24h, with solution dilution and vacuum filtration, washing and filtering was neutral back 50 ℃ of vacuum-drying 24h until carbon nanotube pH value repeatedly after backflow finished;
Step 2: the multi-walled carbon nano-tubes that concentrated nitric acid oxidation is handled is inserted round-bottomed flask; The dry toluene of crossing of anhydrous calciumsulphate is added in the flask in the ratio with carbon nanotube 1g: 20mL; After stirring at normal temperature solution mixes trimethylchlorosilane solution is added in the ratio with toluene 1mL: 10mL fast, and seal bottleneck normal temperature mixing 10min, with 90 ℃ of oil bath reflux of the solution that mixes 24h with glass stopper; After backflow finishes solution for vacuum is filtered; And, be neutral until material pH value, at last with 50 ℃ of vacuum-drying 24h of material with toluene and zero(ppm) water washing and filtering repeatedly.
The present invention proposes the method that surface-treated multi-walled carbon nano-tubes and the high surface tension liquid of polarity is combined into a kind of novel nano fluid power consumption material; Solid through overcoming---liquid capillary force and interfacial force acting; The mechanical energy of extraneous input has effectively dissipated; And the cost of material is low, need not the external world driving energy is provided.
Description of drawings
Fig. 1 is a nano-fluid material compression testing device synoptic diagram;
Fig. 2 is an I class nano-fluid material power consumption graphic representation;
Fig. 3 is an II class nano-fluid material power consumption graphic representation.
Embodiment
For example the present invention is described further below in conjunction with accompanying drawing.
Embodiment 1: power consumption nano-fluid material of the present invention is to form like this: length is that nano level multi-walled carbon nano-tubes is at the pipe inside and outside wall; Mouth of pipe grafting trimethyl silane functional group particularly; The high surface tension liquid of the supporting use polarity of the multi-walled carbon nano-tubes of grafting trimethyl silane functional group; The high surface tension liquid of polarity must can not be soaked into the multi-walled carbon nano-tubes after handling each other, adopts the contact angle of the multi-wall carbon nano-tube tube-surface of measurement liquid after processing and the method for roll angle to select the high surface tension liquid of polarity; The multi-walled carbon nano-tubes powder constituent of water or terepthaloyl moietie or USP Kosher and grafting trimethyl silane functional group has the nano-fluid material of energy dissipation capacity.
Power consumption nano-fluid preparation methods of the present invention, step is following:
Step 1: with diameter less than 8nm; Purity is 68% the concentrated nitric acid mixed by 1g: 100mL greater than 95% multi-walled carbon nano-tubes and concentration; The normal temperature lower magnetic force stirs 10min; Pour mixed solution into 100 ℃ of oil bath reflux of round-bottomed flask 24h, with solution dilution and vacuum filtration, washing and filtering was neutral back 50 ℃ of vacuum-drying 24h until carbon nanotube pH value repeatedly after backflow finished;
Step 2: the multi-walled carbon nano-tubes that concentrated nitric acid oxidation is handled is inserted round-bottomed flask; The dry toluene of crossing of anhydrous calciumsulphate is added in the flask in the ratio with carbon nanotube 1g: 20mL; After stirring at normal temperature solution mixes trimethylchlorosilane solution is added in the ratio with toluene 1mL: 10mL fast, and seal bottleneck normal temperature mixing 10min, with 90 ℃ of oil bath reflux of the solution that mixes 24h with glass stopper; After backflow finishes solution for vacuum is filtered; And, be neutral until material pH value, at last with 50 ℃ of vacuum-drying 24h of material with toluene and zero(ppm) water washing and filtering repeatedly.
Embodiment 2: combine Fig. 1, the present invention nano-fluid material that consumes energy to be made up of the multi-walled carbon nano-tubes and the high surface tension liquid of polarity (water or USP Kosher) of surface grafting trimethyl silane functional group.The carbon nanotube that at present domestic many carbon nanotube manufacturer can provide oxidized activating to cross, but cause the content of carbon nanotube grafted carboxyl and hydroxyl low because general degree of oxidation is low, influence the percentage of grafting of trimethyl silane functional group.Simultaneously because SWCN grafting process can not guarantee that functional group is in the chamber, thus the present invention to select purity for use be that 95% multi-walled carbon nano-tubes carries out oxidized activating and handles.The carbon nano tube surface treatment process is: be 68% the concentrated nitric acid mixed by 1g: 100mL less than the multi-walled carbon nano-tubes of 8nm and concentration with diameter, the normal temperature lower magnetic force stirs 10min.Pour mixed solution into 100 ℃ of oil bath reflux of round-bottomed flask 24h.After backflow finishes solution is added a large amount of distilled water diluting final vacuums and filter, washing and filtering is neutral until carbon pipe pH value repeatedly, 50 ℃ of vacuum-drying 24h.The multi-walled carbon nano-tubes of oxide treatment is inserted round-bottomed flask, add the ratio of the dry toluene of crossing of anhydrous calciumsulphate in the flask in 1g: 20mL.After stirring at normal temperature solution mixes with trimethylchlorosilane solution in adding fast with the ratio of toluene in 1mL: 10mL, and seal bottleneck normal temperature mixing 10min with glass stopper.With 90 ℃ of oil bath reflux of the solution that mixes 24h.The backflow back solution for vacuum that finishes is filtered, and with toluene and zero(ppm) water washing and filtering repeatedly, is neutrality until material pH value, at last with 50 ℃ of vacuum-drying 24h of material.
The high surface tension liquid of polarity of forming the power consumption nano-fluid must satisfy with handle after the condition that can not soak into each other of multi-walled carbon nano-tubes, the present invention adopt measure solid---the method for liquid surface contact angle and roll angle is sought suitable liquid.All can form 120 °-150 ° contact angle through high surface tension liquid of various polarity such as evidence water, terepthaloyl moietie, USP Kosher with the multi-wall carbon nano-tube pipe powder of grafting trimethyl silane functional group; Solid-liquid can not soak into each other, can form power consumption nano-fluid material.
In order to verify the energy dissipation capacity of this nano-fluid, the present invention has designed a kind of simple liquid compressing device.With surface-treated multi-walled carbon nano-tubes 1g with put into hydraulic tank after 10g zero(ppm) water mixes and carry out applied voltage test.Because the water capacity is prone to cause the corrosion of container to damage, for the ease of the application of this nano-fluid, the equally just surface-treated multi-walled carbon nano-tubes 1g of the present invention with put into hydraulic tank after the 10g USP Kosher mixes and carry out applied voltage test.Evidence: the nano-fluid material that utilizes the present invention to prepare is once adding the bigger hysteresis area of unloading back formation; For example fluid overcomes solid when outside pressure reaches 3MPa---and the liquid capillary force gets in the carbon nanotube; Form stress plateau, have stronger energy dissipation capacity.
Embodiment 3: combine Fig. 1, Fig. 2, Fig. 3, nano-fluid power consumption test set is as shown in Figure 1, and whole testing device is made up of pressurizing piston and cylinder body.Piston is made up of No. 45 steel of chromium plating annealing, and diameter is 20mm, and length is 70mm, and the piston upstream end uses the reinforced TFE coating parcel of thickness as 1mm.The hydraulic seal cylinder body is made up of modified No. 45 steel of normalizing, and cylinder diameter is 22mm, and external diameter is 38mm.In order to prevent liquid seepage under the High Voltage effect in the cylinder, the hydro-cylinder top is provided with the thick sealing rubber ring of 5mm respectively and 2 road thickness are the reinforced TFE Seal Kit of 1mm.For at the front-seat gas in the jar that removes of liquid pressurization, the vent valve that it is 1mm that the hydro-cylinder bottom is provided with one diameter, this vent valve also is used for the piston that is pressed in the cylinder is ejected.
The mixing liquid of surface-treated multi-walled carbon nano-tubes and water or USP Kosher is poured in the hydro-cylinder, adopted Ins tron 5569 universal testing machines that piston is pressed in the cylinder.In order to avoid the frictional force influence of piston and hydro-cylinder as far as possible, trier loads and adopts the displacement control method, and loading velocity is 1mm/min, and loading environment can be considered intends the static(al) loading.When pressure in the cylinder reaches the required highest pressure of test,, accomplish once to add unloading experiment with the speed unloading of trier with 1mm/min.Add the nano-fluid that water is formed for carbon nanotube, carbon nanotube was because the duct contains air before material loaded, and carbon nanotube all swims on the water surface.Once add unloading rear section carbon nanotube and get in the water, form suspension-s, part is suspended on the water surface owing to water in the pipe is discharged again.Add the nano-fluid that USP Kosher is formed for carbon nanotube,, carbon nanotube is added the back vigorous stirring, even carbon nanotube is scattered in the USP Kosher because the USP Kosher viscosity is bigger.Once add unloading back carbon nanotube and still be dispersed in the USP Kosher, rear section carbon nanotube of static for some time floats on the USP Kosher surface again.
The nano-fluid material energy dissipation capacity that Fig. 2 forms for the multi-walled carbon nano-tubes and the water of employing test set test surfaces grafting trimethyl silane shown in Figure 1 functional group.The preparation method of the multi-walled carbon nano-tubes of surface grafting trimethyl silane functional group is: be 68% the concentrated nitric acid mixed by 1g: 100mL less than the multi-walled carbon nano-tubes of 8nm and concentration with diameter, the normal temperature lower magnetic force is poured mixed solution into 100 ℃ of oil bath reflux of round-bottomed flask 24h after stirring 10min.After backflow finishes solution is added a large amount of distilled water diluting final vacuums and filter, dilute filtration is neutral until carbon nanotube pH value repeatedly, 50 ℃ of vacuum-drying 24h.Multi-walled carbon nano-tubes after the concentrated nitric acid oxidation processing is inserted round-bottomed flask, the ratio of the dry toluene of crossing of anhydrous calciumsulphate in 1g: 20mL added in the flask.After stirring at normal temperature solution mixes trimethylchlorosilane solution is added in the ratio with toluene 1mL: 10mL fast, and clog bottleneck normal temperature mixing 10min with glass stopper.With 90 ℃ of oil bath reflux of the solution that mixes 24h.After backflow finishes solution for vacuum is filtered, and, be neutrality until material pH value, at last with 50 ℃ of vacuum-drying 24h of material with toluene and zero(ppm) water washing and filtering repeatedly.
The static contact angle of the multi-walled carbon nano-tubes after test zero(ppm) water and the surface treatment is greater than 90 °, and two kinds of materials can not soak into each other, therefore can select water to form the nano-fluid material as fluid and surface-treated carbon nanotube.
As can be seen from Figure 2, this nano-fluid is under the low pressure effect, and fluid can't overcome capillary force and get in the carbon nanotube road, and the curve initial stage is the compression of water.When pressure reached 3MPa in the cylinder, water molecules began to get in the more weak carbon nanotube road of some capillary force.Along with the further rising of pressure, water molecules progressively gets in the stronger carbon nanotube road of capillary force, forms the stress plateau of similar steel viscous deformation.When pressure reached 6MPa, all carbon nanotubes were all occupied by water molecules, and curve becomes the compression process of water again.When pressure reaches 20MPa in the cylinder, begin unloading, this moment, curve was undertaken by the unloading manner of zero(ppm) water, and wherein the part water molecules flows out from the carbon nanoporous.Add unloading curve and formed a similar orthogonal envelope area, the energy with regard to obtaining this nano-fluid material dissipation of finding the solution this area is about 3J/g.
Fig. 3 puts into the test set shown in Figure 1 test of consuming energy with the nano-fluid material that the multi-walled carbon nano-tubes of surface grafting trimethyl silane functional group and USP Kosher are formed.Fig. 3 has shown that equally Fig. 2's adds the unloading rule.Because Fig. 3 fluid has adopted and the water ratio, the USP Kosher that viscosity is big, surface tension is little, the pressure that the fluid that therefore obtains gets into carbon nanotube is 2MPa, the stress plateau shape is also different simultaneously.This material adds unloading curve and has formed a similar orthogonal envelope area equally, and the energy with regard to obtaining this nano-fluid material dissipation of finding the solution this area is about 2.5J/g.
Through experimental study, it is considered herein that influencing the principal element that fluid gets into the minimum pressure P of carbon nanotube is: carbon nanotube caliber size, solid---surface tension between liquid is poor, functional group's proterties at nanoporous road junction, adopt fluidic each item character etc.
Claims (2)
1. power consumption nano-fluid material; It is characterized in that: length is that nano level multi-walled carbon nano-tubes is at the pipe inside and outside wall; Mouth of pipe grafting trimethyl silane functional group; The high surface tension liquid of the supporting use polarity of the multi-walled carbon nano-tubes of grafting trimethyl silane functional group, the high surface tension liquid of polarity must can not be soaked into the multi-walled carbon nano-tubes after handling each other, adopts the contact angle of the multi-wall carbon nano-tube tube-surface of measurement liquid after processing and the method for roll angle to select the high surface tension liquid of polarity; The multi-walled carbon nano-tubes powder constituent of water or terepthaloyl moietie or USP Kosher and grafting trimethyl silane functional group has the nano-fluid material of energy dissipation capacity.
2. the preparation method of the multi-wall carbon nano-tube pipe powder of a grafting trimethyl silane functional group, it is characterized in that: step is following:
Step 1: with diameter less than 8nm; Purity is 68% the concentrated nitric acid mixed by 1g: 100mL greater than 95% multi-walled carbon nano-tubes and concentration; The normal temperature lower magnetic force stirs 10min; Pour mixed solution into 100 ℃ of oil bath reflux of round-bottomed flask 24h, with solution dilution and vacuum filtration, washing and filtering was neutral back 50 ℃ of vacuum-drying 24h until carbon nanotube pH value repeatedly after backflow finished;
Step 2: the multi-walled carbon nano-tubes that concentrated nitric acid oxidation is handled is inserted round-bottomed flask; The dry toluene of crossing of anhydrous calciumsulphate is added in the flask in the ratio with carbon nanotube 1g: 20mL; After stirring at normal temperature solution mixes trimethylchlorosilane solution is added in the ratio with toluene 1mL: 10mL fast, and seal bottleneck normal temperature mixing 10min, with 90 ℃ of oil bath reflux of the solution that mixes 24h with glass stopper; After backflow finishes solution for vacuum is filtered; And, be neutral until material pH value, at last with 50 ℃ of vacuum-drying 24h of material with toluene and zero(ppm) water washing and filtering repeatedly.
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| CN101010259A (en) * | 2004-06-01 | 2007-08-01 | 奇梦达股份公司 | Silanized carbon nanotubes and method for the production thereof |
| CN101469141A (en) * | 2007-12-28 | 2009-07-01 | 中国科学院兰州化学物理研究所 | Method for preparing multi-wall carbon nano-tube composite material |
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| CN101010259A (en) * | 2004-06-01 | 2007-08-01 | 奇梦达股份公司 | Silanized carbon nanotubes and method for the production thereof |
| CN101469141A (en) * | 2007-12-28 | 2009-07-01 | 中国科学院兰州化学物理研究所 | Method for preparing multi-wall carbon nano-tube composite material |
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