CN102060286A - 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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- CN102060286A CN102060286A CN 201010541578 CN201010541578A CN102060286A CN 102060286 A CN102060286 A CN 102060286A CN 201010541578 CN201010541578 CN 201010541578 CN 201010541578 A CN201010541578 A CN 201010541578A CN 102060286 A CN102060286 A CN 102060286A
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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
(1) technical field
The present invention relates to Materials science, is exactly a kind of power consumption nano-fluid material and preparation method thereof specifically.
(2) 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 has been subjected to 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 Single Walled Carbon Nanotube.Studies show that though carbon nanotube itself is a hydrophobic material, water molecules can flow into automatically and by carbon nanotube, behind the Van der Waals force between reduction tube wall and water molecules, water molecules can not enter and pass through carbon nanotube.People such as J.A.Thomasa utilize computer 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.Studies show 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 by Chinese scholars fits experiment as can be known, though carbon nanotube itself is a hydrophobic material, if do not carry out surface treatment, water molecules can enter automatically and by 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.
(3) 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 object of the present invention is achieved 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 mutually with the multi-walled carbon nano-tubes after handling, and 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 ethylene glycol or glycerol and grafting trimethyl silane functional group has the nano-fluid material of energy dissipation capacity.
Described power consumption nano-fluid preparation methods, step is as follows:
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 the 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 fast in the ratio with toluene 1mL: 10mL, and seal bottleneck normal temperature mixing 10min with glass stopper, with 90 ℃ of oil bath reflux of the solution 24h that mixes, after backflow finishes solution for vacuum is filtered, and with toluene and distilled water washing and filtering repeatedly, until the material pH value is neutral, at last with 50 ℃ of vacuum-drying 24h of material.
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 by 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.
(4) 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.
(5) embodiment
The invention will be further described for example 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 mutually with the multi-walled carbon nano-tubes after handling, and 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 ethylene glycol or glycerol 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 as follows:
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 the 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 fast in the ratio with toluene 1mL: 10mL, and seal bottleneck normal temperature mixing 10min with glass stopper, with 90 ℃ of oil bath reflux of the solution 24h that mixes, after backflow finishes solution for vacuum is filtered, and with toluene and distilled water washing and filtering repeatedly, until the material pH value is neutral, at last with 50 ℃ of vacuum-drying 24h of material.
Embodiment 2: in conjunction with Fig. 1, the present invention's nano-fluid material that consumes energy is made up of the multi-walled carbon nano-tubes and the high surface tension liquid of polarity (water or glycerol) 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 Single Walled Carbon Nanotube 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, 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 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 24h that mixes.The backflow back solution for vacuum that finishes is filtered, and with toluene and distilled water washing and filtering repeatedly, is neutrality until the 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 mutually 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, ethylene glycol, glycerol with the multi-wall carbon nano-tube pipe powder of grafting trimethyl silane functional group, solid-liquid can not soak into mutually, 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 distilled water mixes and carry out applied voltage test.Because the water capacity easily causes 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 glycerol is mixed 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 enters in the carbon nanotube, form stress plateau, have stronger energy dissipation capacity.
Embodiment 3: in conjunction with Fig. 1, Fig. 2, Fig. 3, nano-fluid consumes energy test set as shown in Figure 1, and whole testing device is made up of pressurizing piston and cylinder body.Piston is made of No. 45 steel of chromium plating annealing, and diameter is 20mm, and length is 70mm, and piston upstream end thickness is the reinforced TFE coating parcel of 1mm.The hydraulic seal cylinder body is made 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, the piston that this vent valve also is used for being pressed in the cylinder ejects.
The mixing liquid of surface-treated multi-walled carbon nano-tubes and water or glycerol is poured in the hydro-cylinder, adopted Instron 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,, finish 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 enter in the water, form suspension, part is suspended on the water surface again owing to water in the pipe is discharged.Add the nano-fluid that glycerol is formed for carbon nanotube,, carbon nanotube is added the back vigorous stirring, even carbon nanotube is scattered in the glycerol because the glycerol viscosity is bigger.Once add unloading back carbon nanotube and still be dispersed in the glycerol, rear section carbon nanotube of static for some time floats on the glycerol 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 the 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 fast in the ratio with toluene 1mL: 10mL, and clog bottleneck normal temperature mixing 10min with glass stopper.With 90 ℃ of oil bath reflux of the solution 24h that mixes.After backflow finishes solution for vacuum is filtered, and, be neutrality until the material pH value, at last with 50 ℃ of vacuum-drying 24h of material with toluene and distilled water washing and filtering repeatedly.
The static contact angle of the multi-walled carbon nano-tubes after test distilled water and the surface treatment is greater than 90 °, and two kinds of materials can not soak into mutually, therefore can select water as fluid and surface-treated carbon nanotube composition nano-fluid material.
As can be seen from Figure 2, this nano-fluid is under the low pressure effect, and fluid can't overcome capillary force and enter 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 enter in the more weak carbon nanotube road of some capillary force.Along with the further rising of pressure, water molecules progressively enters 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.Begin unloading when pressure reaches 20MPa in the cylinder, this moment, curve was undertaken by the unloading manner of distilled water, and wherein the portion water molecule 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 glycerol are formed.Fig. 3 has shown that equally Fig. 2's adds the unloading rule.Because Fig. 3 fluid adopted and the water ratio, the glycerol that viscosity is big, surface tension is little, therefore to enter the pressure of carbon nanotube be 2MPa to the fluid that obtains, 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.
Research by experiment it is considered herein that influence the principal element that fluid enters 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, the every character of employing fluidic 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 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 mutually with the multi-walled carbon nano-tubes after handling, and 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 ethylene glycol or glycerol and grafting trimethyl silane functional group has the nano-fluid material of energy dissipation capacity.
2. power consumption nano-fluid preparation methods as claimed in claim 1, it is characterized in that: step is as follows:
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 the 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 fast in the ratio with toluene 1mL: 10mL, and seal bottleneck normal temperature mixing 10min with glass stopper, with 90 ℃ of oil bath reflux of the solution 24h that mixes, after backflow finishes solution for vacuum is filtered, and with toluene and distilled water washing and filtering repeatedly, until the material pH value is neutral, at last with 50 ℃ of vacuum-drying 24h of material.
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| CN109135686A (en) * | 2018-08-10 | 2019-01-04 | 中国矿业大学 | A kind of graphene-based modified Nano fluid heat transferring working medium and preparation method thereof |
Citations (3)
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|---|---|---|---|---|
| WO2005012171A2 (en) * | 2003-07-28 | 2005-02-10 | William Marsh Rice University | Sidewall functionalization of carbon nanotubes with organosilanes for polymer composites |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005012171A2 (en) * | 2003-07-28 | 2005-02-10 | William Marsh Rice University | Sidewall functionalization of carbon nanotubes with organosilanes for polymer composites |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135686A (en) * | 2018-08-10 | 2019-01-04 | 中国矿业大学 | A kind of graphene-based modified Nano fluid heat transferring working medium and preparation method thereof |
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