CN102505574A - Intelligent energy-saving graphene oxide composite paper and preparation method thereof - Google Patents
Intelligent energy-saving graphene oxide composite paper and preparation method thereof Download PDFInfo
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Abstract
The invention discloses intelligent energy-saving graphene oxide composite paper and a preparation method thereof, wherein the intelligent energy-saving graphene oxide composite paper is obtained by layer-by-layer self-assembly of graphene oxide and an organic phase change material; the addition amount of the organic phase change material is 1-85% of the mass of the intelligent energy-saving graphene oxide composite paper; and the rest is graphene oxide. The graphene oxide composite paper provided in the invention can prevent the organic phase change material from leakage effectively and improve heat conductivity; and the method is simple in operation and low in cost, can be finished in a common chemical laboratory, and is easy to popularize. The intelligent energy-saving graphene oxide composite paper prepared by the method has strong flexibility and variable phase change temperature and meets different application requirements, such as thermal interface materials of electronic devices, etc., and the material has a wide application prospect.
Description
One, technical field
The present invention relates to a kind of preparation of nanomaterials, specifically a kind of intelligent power saving graphene oxide composite sheet and preparation method thereof.
Two, background technology
The energy and environment are the most challenging two large problems of 21 century face of mankind.In the energy development strategic plan that formulate countries in the world, develop reproducible new forms of energy and rationally utilize existing non-renewable energy resources to occupy same status.And save existing non-renewable energy resources are cores that reasonable energy utilization is paid close attention to by people most, and energy-conservation level is to weigh the important symbol of a national science technology, the advanced degree of industrial level.
Efficiently utilizing heat energy is one of energy-saving and cost-reducing middle key issue.This is that in the utilization of the various energy, 85-90% is through converting the demand that heat energy satisfies people to because heat energy is type of service the most widely in the using energy source always.And one of the waste of heat energy, inefficient use difficult problem that to be countries in the world need to be resolved hurrily always.2002, U.S. statistics showed that the various utilization efficiency of energy of this state have only 42%, and in 58% energy waste, major part is that the form with heat is not intended to the free burial ground for the destitute and has been dissipated.
Energy-saving field, intelligent power saving are the main flow directions of current development.So-called intelligent power saving is meant that environment carries out perception to external world, through oneself's adjusting, controllably absorbs outside energy and discharges self-energy, the purpose of reach high efficiency, reasonably utilizing energy, cut down the consumption of energy.Its core material is called the intelligent power saving material.This adjustable intellectual material is the target that current energy-saving field people pursue, and is the basis with the intelligent power saving material, and the intelligent power saving technology of development is the forward position of this area research.Utilize the closely-related light of material and natural environment, hot alert and resourceful characteristic; Construct the intelligent power saving system; Being the mainstream development direction of building energy saving field, also is one of important selection and goal in research of realizing the interior temperature adjustings of other field envelopes such as automobile and aerospaceplane.
Utilize material energy-absorbing and the characteristics of releasing ability in phase transition process, realize that the storage of energy and utilization are in recent years in one of active direction of various fields such as the energy, material, Aero-Space, weaving, electric power, medical instrument, building.Phase-change accumulation energy has advantages such as energy storage density height, energy storage easy control of temperature and range of choice are wide, has got into practicability and commercialization stage in some fields at present.The phase-changing energy storage material kind is a lot.Attempt adopting phase-changing energy storage material to reduce building energy consumption in fields such as buildings long history has been arranged.But itself be prone to leak, encapsulation require high, be prone to shortcomings such as aging, limited its application in the dissipation from electronic devices field.On the other hand, lower thermal conductivity is the another one technical bottleneck problem of restriction organic phase-change heat accumulating large-scale promotion application.Therefore the advantage that combines two kinds of phase transformations; People have been developed shaping phase-change material; Improved the performance of phase-change heat-storage material to a certain extent, but still there is the problem of aspects such as encapsulation in traditional shaping phase-change material in practical application, can't fundamentally changes the shortcoming of above-mentioned two kinds of systems.
Graphene oxide; Be by behind the graphite chemical oxidation; Through the ultrasonic a kind of novel carbon nanomaterial that obtains of peeling off, the parent who more and more receives people because it has the characteristic of good electronics, mechanical performance and light-high-strength looks at, and is widely used in material science.Graphene oxide has been owing to introduced oxy radicals such as hydroxyl, carboxyl and epoxy radicals on the big conjugate surface of Graphene, thereby is prone to and H
2Hydrogen bond actions such as O form the Graphene paper of micro-nano thickness.People such as Dikin D.A. have reported the preparation and the sign of graphene oxide paper on " Nature " in 2007, in addition, people such as Zhu Y.W. also reported the preparation of transparent graphene oxide film at " Appl.Phys.Lett. " in 2009.Therefore, utilize graphene oxide to be prone to process the characteristics of paper, people such as Putz K.W. have synthesized high-intensity graphene oxide/polymer thin-film material at " Adv.Funct.Mater. " report in 2010.So, utilize characteristics that graphene oxide is prone to process paper for the preparation shaping phase-change material provide maybe, prepare simultaneously that a kind of to have intelligent power saving graphene oxide paper be that the efficient utilization of heat energy provides good material system.
Three, summary of the invention
The objective of the invention is to require shortcomings such as height, easy aging, low thermal conductance for the easy leakage, the encapsulation that overcome organic phase change material; Aim to provide intelligent power saving graphene oxide composite sheet of a kind of fixed phase change and preparation method thereof, thereby obtain the intelligent power saving graphene oxide composite sheet material of different phase transition temperatures.
Technical solution problem of the present invention adopts following technical scheme:
The characteristics of intelligent power saving graphene oxide composite sheet of the present invention are: said intelligent power saving graphene oxide composite sheet is obtained through self assembly layer by layer by graphene oxide and organic phase change material; Wherein the addition of organic phase change material is the 1-85% of said intelligent power saving graphene oxide composite sheet quality, and surplus is a graphene oxide;
Said organic phase change material is fatty alcohol and aliphatic acid etc.
The characteristics of intelligent power saving graphene oxide composite sheet of the present invention also are: said fatty alcohol is selected from polyethylene glycol or positive tetradecyl alchohol.
The characteristics of intelligent power saving graphene oxide composite sheet of the present invention also are: said polyethylene glycol is PEG400, PEG600, PEG2000 or PEG20000.
The characteristics of intelligent power saving graphene oxide composite sheet of the present invention also are: said aliphatic acid is selected from stearic acid, laurate or palmitic acid.
The preparation method's of intelligent power saving graphene oxide composite sheet of the present invention characteristics are may further comprise the steps:
The preparation of a, graphite oxide
0.6-1g graphite is placed the concentrated sulfuric acid, the 1gK of 200mL mass concentration 98%
2S
2O
8And 1gP
2O
5Mixed solution in 85-90 ℃ of reaction 4.5 hours, reaction back is with 200mL deionized water dilute reaction solution, successively through filtration, wash and 60 ℃ of vacuumizes after obtain graphite oxide;
The preparation of b, graphene oxide
The concentrated sulfuric acid and the 1gKMnO that in the graphite oxide that 50mg step a obtains, add 20-25mL mass concentration 98%
4In 30-40 ℃ of reaction 2 hours; In reactant liquor, add the 20mL deionized water then and continue reaction 0.5 hour in 95 ℃, add the hydrogen peroxide solution cessation reaction of 3mL mass concentration 30% subsequently, after centrifugal, washing and 30-40 ℃ of vacuumize, obtain graphene oxide successively;
Said washing is a HCl solution washing of using deionized water and mass concentration 10% respectively;
The preparation of c, intelligent power saving graphene oxide composite sheet
With water or DMF is solvent; Get the dried graphene oxide of 20mg; Obtain the favorable dispersibility graphene oxide through behind the ultrasonic 30min; Mix with organic phase change material again,, separate the back with filter membrane and promptly get intelligent power saving graphene oxide composite sheet 30-40 ℃ of vacuumize through ultrasonic 30min final vacuum suction filtration;
The time 0.5-1 of ultrasonic dispersion among the said step c hour.
Compared with present technology, beneficial effect of the present invention is embodied in:
1, the present invention with graphene oxide with after organic phase change material mixes; Utilize the vacuum self-assembling technique graphene oxide and phase-change material to be adopted the self assembly of layer-by-layer; Thereby obtain to have the graphene oxide composite sheet of energy saving effect; Can be good at preventing the leakage, aging of organic phase change material, and improved performance such as thermal conductance; And the report of Wang W.L. scientific research group on 2009 " Applied Energy " in the prior art adopts expanded graphite and polyethylene glycol (PEG) method of mixing to obtain energy storage material.But the material that this simple employing method of mixing obtains, polyethylene glycol mixes inhomogeneous with expanded graphite, influence the thermal conductivity of material.
2, the present invention can be used as phase-change material to obtain the graphene oxide composite sheet of different phase transition temperature interval through fatty alcohol or the aliphatic acid that uses different carbon chain lengths; Along with the polyethylene glycol number-average molecular weight increases to 20000 from 600; The hot temperature of storing of graphene oxide composite sheet also changes thereupon; As the graphene oxide composite sheet of the Macrogol 600 that mixes heat absorption heat accumulation temperature is about 18～22 ℃, the graphene oxide composite sheet heat absorption heat accumulation temperature of doping Macrogol 2000 and is about 41～46 ℃, the graphene oxide composite sheet heat absorption heat accumulation temperature of doping Macrogol 2000 0 and is about 60～62 ℃, can satisfy the needs that different temperatures is required.
3, compare with traditional organic phase change material, intelligent power saving graphene oxide composite sheet material of the present invention also has good flexibility characteristics, can also be cut into different shapes, can also be widely used in the thermal interfacial material of electronic device.
4, the present invention is simple to operate, and cost is low, all can accomplish at general chemical laboratory, is easy to promote.
Four, description of drawings
Fig. 1 is the optical photograph of the intelligent power saving graphene oxide composite sheet of the inventive method preparation.Letter " IIM " becomes more and more fuzzyyer with the graphene oxide composite sheet of different-thickness among Fig. 1, until covering fully.
Fig. 2 is the scanning electron microscope diagram of the intelligent power saving graphene oxide composite sheet of the inventive method preparation.As can be seen from Figure 2 the thickness of graphene oxide composite sheet can be accomplished 10 microns to up to a hundred microns (Fig. 2 (A), (B)).Simultaneously; The stereoscan photograph (Fig. 2 (C)) that high power is amplified can find out that the graphene oxide composite sheet is to be formed by graphene oxide and organic phase change material self assembly layer by layer, has confirmed that thus the graphene oxide composite sheet is to adopt the self assembly of layer-by-layer method to form.
Fig. 3 is the infrared spectrum of the intelligent power saving graphene oxide composite sheet of the inventive method preparation.Can clearly find out that from Fig. 3 hydrocarbon key peak position is at 3000-2700cm in methyl and the methylene
-1Between the position.The peak position value of this infrared spectrum shows the self assembly of phase-change material and graphene oxide.
Fig. 4 is the dissociated optical photo of the intelligent power saving graphene oxide composite sheet of the inventive method preparation.Can find out that from photo graphene oxide composite sheet of the present invention is easy to strip down.
Fig. 5 is the curved optical photo of the intelligent power saving graphene oxide composite sheet of the inventive method preparation.Can find out that from photo graphene oxide composite sheet of the present invention has good flexible.
Fig. 6 is a kind of intelligent power saving graphene oxide/four circulative DSC figure of polyethylene glycol PEG2000 composite sheet of the inventive method preparation.As can be seen from the figure, graphene oxide composite sheet of the present invention has good heat absorption exothermicity, and the recycling of heat absorption heat release is worth very high.
Five, the specific embodiment:
Come technical scheme of the present invention is described further below in conjunction with specific embodiment.
Embodiment 1:
Intelligent power saving graphene oxide composite sheet is obtained through self assembly layer by layer by graphene oxide and organic phase change material PEG2000 in the present embodiment, and wherein the quality of organic phase change material PEG2000 is 20mg, and the quality of graphene oxide is 20mg.
Intelligent power saving graphene oxide composite sheet prepares by following method in the present embodiment:
0.8g graphite is placed the concentrated sulfuric acid, the 1gK of 200mL mass concentration 98%
2S
2O
8And 1gP
2O
5Mixed solution in 85-90 ℃ of reaction 4.5 hours, reaction back is with 200mL deionized water dilute reaction solution, successively through filtration, wash and 60 ℃ of vacuumizes after obtain graphite oxide;
The concentrated sulfuric acid and the 1gKMnO that in the 50mg graphite oxide, add 20-25mL mass concentration 98%
4In 30-40 ℃ of reaction 2 hours; In reactant liquor, add the 20mL deionized water then and continue reaction 0.5 hour in 95 ℃, add the hydrogen peroxide solution cessation reaction of 3mL mass concentration 30% subsequently, successively through centrifugal, washing with after 30-40 ℃ of vacuumize, obtain graphene oxide;
Get the dry graphene oxide of 20mg, add 20mL water, obtain the favorable dispersibility graphene oxide through behind the ultrasonic 30min; Get 20mg PEG2000, add 20mL water, behind the ultrasonic 30min PEG2000 solution is added in the graphene oxide; And then ultrasonic 10-20min gets mixed solution; Adopt water-based miillpore filter (diameter: 50mm, aperture: 0.22 μ m), drain after 36 hours with gained mixed solution vacuum filtration;
Filter cake dry 30min under 40 ℃ with vacuum filtration peel off after the taking-up with filter membrane and separate, and then drying can obtain intelligent power saving graphene oxide composite sheet in 6 hours in 40 ℃ baking oven.
Embodiment 2:
The present embodiment preparation method is with embodiment 1, and different is that organic phase change material is PEG400, and addition is respectively 5mg, 15mg, 20mg and 113mg.
Embodiment 3:
The present embodiment preparation method is with embodiment 1, and different is that organic phase change material is PEG600, and addition is respectively 5mg, 15mg, 17mg and 20mg.
Embodiment 4:
The present embodiment preparation method is with embodiment 1, and different is that organic phase change material is PEG2000, and addition is respectively 5mg, 15mg, 17mg and 20mg.
Embodiment 5:
The present embodiment preparation method is with embodiment 1, and the addition of different is PEG2000 is respectively and is 5mg, 15mg and 113mg.
Embodiment 6:
Intelligent power saving graphene oxide composite sheet is obtained through self assembly layer by layer by graphene oxide and organic phase change material stearic acid in the present embodiment, and wherein the quality of organic phase change material is 20mg, and the quality of graphene oxide is 20mg.
Intelligent power saving graphene oxide composite sheet prepares by following method in the present embodiment:
0.8g graphite is placed the concentrated sulfuric acid, the 1gK of 200mL mass concentration 98%
2S
2O
8And 1gP
2O
5Mixed solution in 85-90 ℃ of reaction 4.5 hours, reaction back is with 200mL deionized water dilute reaction solution, successively through filtration, wash and 60 ℃ of vacuumizes after obtain graphite oxide;
The concentrated sulfuric acid and the 1gKMnO that in the 50mg graphite oxide, add 20-25mL mass concentration 98%
4In 30-40 ℃ of reaction 2 hours; In reactant liquor, add the 20mL deionized water then and continue reaction 0.5 hour in 95 ℃, add the hydrogen peroxide solution cessation reaction of 3mL mass concentration 30% subsequently, successively through centrifugal, washing with after 30-40 ℃ of vacuumize, obtain graphene oxide;
Get the dry graphene oxide of 20mg, add the 20mL dry DMF, through obtaining the graphene oxide of favorable dispersibility behind the ultrasonic 30min; Get the 20mg stearic acid and add the 20mL dry DMF; Behind the ultrasonic 30min stearic solution is added in the graphene oxide of favorable dispersibility; And then ultrasonic 10-20min gets mixed solution; Adopt organic miillpore filter (diameter: 50mm, aperture: 0.45 μ m), drain after 36 hours with gained mixed solution vacuum filtration;
Filter cake dry 30min under 40 ℃ with vacuum filtration peel off after the taking-up with filter membrane and separate, and then drying can obtain intelligent power saving graphene oxide composite sheet in 6 hours in 40 ℃ baking oven.
Embodiment 7:
The present embodiment preparation method is with embodiment 6, and different is that organic phase change material is a laurate, and addition is respectively 5mg, 15mg, 20mg and 113mg.
Embodiment 8:
The present embodiment preparation method is with embodiment 6, and different is that organic phase change material is a palmitic acid, and addition is respectively 5mg, 15mg, 17mg and 20mg.
Embodiment 9:
The present embodiment preparation method is with embodiment 1, and different is that organic phase change material is a stearic acid, and addition is respectively 5mg, 15mg and 113mg.
Claims (6)
1. intelligent power saving graphene oxide composite sheet; It is characterized in that: said intelligent power saving graphene oxide composite sheet is obtained through self assembly layer by layer by graphene oxide and organic phase change material; Wherein the addition of organic phase change material is the 1-85% of said intelligent power saving graphene oxide composite sheet quality, and surplus is a graphene oxide;
Said organic phase change material is fatty alcohol, aliphatic acid or paraffin.
2. intelligent power saving graphene oxide composite sheet according to claim 1 is characterized in that: said fatty alcohol is selected from polyethylene glycol or positive tetradecyl alchohol.
3. intelligent power saving graphene oxide composite sheet according to claim 2 is characterized in that: said polyethylene glycol is PEG400, PEG600, PEG2000 or PEG20000.
4. intelligent power saving graphene oxide composite sheet according to claim 1, it is characterized in that: said aliphatic acid is selected from stearic acid, laurate or palmitic acid.
5. preparation method like claim 1,2,3 or 4 described intelligent power saving graphene oxide composite sheets is characterized in that may further comprise the steps:
The preparation of a, graphite oxide
0.6-1g graphite is placed the concentrated sulfuric acid, the 1gK of 200mL mass concentration 98%
2S
2O
8And 1gP
2O
5Mixed solution in 85-90 ℃ of reaction 4.5 hours, reaction back is with 200mL deionized water dilute reaction solution, successively through filtration, wash and 60 ℃ of vacuumizes after obtain graphite oxide;
The preparation of b, graphene oxide
The concentrated sulfuric acid and the 1gKMnO that in the graphite oxide that 50mg step a obtains, add 20-25mL mass concentration 98%
4In 30-40 ℃ of reaction 2 hours; In reactant liquor, add the 20mL deionized water then and continue reaction 0.5 hour in 95 ℃, add the hydrogen peroxide solution cessation reaction of 3mL mass concentration 30% subsequently, after centrifugal, washing and 30-40 ℃ of vacuumize, obtain graphene oxide successively;
Said washing is a HCl solution washing of using deionized water and mass concentration 10% respectively;
The preparation of c, intelligent power saving graphene oxide composite sheet
With water or DMF is solvent; Get the dry graphene oxide of 20mg, obtain the favorable dispersibility graphene oxide, mix with organic phase change material again through behind the ultrasonic 30min; Through ultrasonic 30min final vacuum suction filtration, separate the back with filter membrane and promptly get intelligent power saving graphene oxide composite sheet 30-40 ℃ of vacuumize.
6. preparation method according to claim 5 is characterized in that: the time 0.5-1 of ultrasonic dispersion among the step c hour.
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| TWI493023B (en) * | 2013-11-21 | 2015-07-21 | Univ Nat Pingtung Sci & Tech | A method for producing a phase change material and the phase change material thereof |
| CN105018041A (en) * | 2015-06-11 | 2015-11-04 | 贵州新碳高科有限责任公司 | Porous graphene film, and phase-changing energy-storing composite material |
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| CN105018041A (en) * | 2015-06-11 | 2015-11-04 | 贵州新碳高科有限责任公司 | Porous graphene film, and phase-changing energy-storing composite material |
| CN105018041B (en) * | 2015-06-11 | 2018-09-11 | 贵州新碳高科有限责任公司 | Graphene porous membrane, phase-change energy-storage composite material |
| CN105112021A (en) * | 2015-07-14 | 2015-12-02 | 中国科学院合肥物质科学研究院 | Energy-saving type three dimensional graphene skeleton composite phase change material with heat storage and release performances, and preparation method thereof |
| CN105018043A (en) * | 2015-07-14 | 2015-11-04 | 中国科学院合肥物质科学研究院 | Use of heat-storage and heat-release graphene composite phase-change material |
| CN105112021B (en) * | 2015-07-14 | 2019-06-18 | 中国科学院合肥物质科学研究院 | A kind of energy-saving three-dimensional graphene framework composite phase-change material and preparation method thereof with heat accumulation exothermicity |
| CN105199675A (en) * | 2015-09-17 | 2015-12-30 | 湖北大学 | Composite phase change material set by oxidized graphene and preparing method thereof |
| CN106255238A (en) * | 2016-02-04 | 2016-12-21 | 济南圣泉集团股份有限公司 | A kind of Graphene thermo electric material and application thereof |
| CN106255238B (en) * | 2016-02-04 | 2019-11-22 | 济南圣泉集团股份有限公司 | A kind of graphene thermo electric material and its application |
| CN106350019A (en) * | 2016-08-18 | 2017-01-25 | 佛山科学技术学院 | Preparation method of composite phase change material based on graphene oxide |
| CN109054761A (en) * | 2018-08-10 | 2018-12-21 | 佛山市中科四维热管理技术有限公司 | A kind of phase-change thermal storage band and preparation method thereof |
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