CN105505330A - Three-dimensional phase-change material based on graphene and preparing method of three-dimensional phase-change material - Google Patents
Three-dimensional phase-change material based on graphene and preparing method of three-dimensional phase-change material Download PDFInfo
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- CN105505330A CN105505330A CN201610049411.9A CN201610049411A CN105505330A CN 105505330 A CN105505330 A CN 105505330A CN 201610049411 A CN201610049411 A CN 201610049411A CN 105505330 A CN105505330 A CN 105505330A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a three-dimensional phase-change material based on graphene and a preparing method of the three-dimensional phase-change material. A graphene oxide aqueous solution with certain concentration is added into liquid nitrogen to be quickly frozen, then graphene oxide aerogel is obtained through freezing drying and is fed into a high-temperature furnace to be subjected to high-temperature heat treatment at 500-3000 DEG C in the inert atmosphere, the treated graphene oxide aerogel is then soaked in dichloromethane solutions with different paraffin concentrations, the product is put into a 30 DEG C vacuum oven to be dried after sufficient absorption, and then the three-dimensional phase-change material based on graphene is obtained. The three-dimensional phase-change material based on graphene is good in paraffin encapsulation effect, the filling amount of paraffin ranges from 0.1% to 99.9%, films and paraffin are uniformly compounded, the melt phase change enthalpy and the solidification phase change enthalpy of the material are basically maintained unchanged after multiple times of heating and cooling circulation, and thus efficient heat energy storage is achieved.
Description
Technical field
The present invention relates to carbon composite phase-change material field, particularly relate to a kind of three-dimensional phase change material based on Graphene and preparation method thereof.
Background technology
Phase change material is that the physical change occurred by temperature variation is carried out absorbing or discharging heat energy.Conventional organic phase change material is due to stable performance, and transformation temperature is wide, and temperature is adjustable etc., and advantage is widely used, but organic phase change material exists heat conductivility difference simultaneously, and volume expansivity is large, easily the shortcoming such as leakage.
Graphene (Graphene) is a kind of unimolecular layer two dimensional crystal, has the intensity that known materials is the highest, and extraordinary specific surface area and the electroconductibility of excellence and thermal conductivity are current optimal two-dimension nano materials.The graphene film of macroscopic view assembling has given full play to graphenic surface and has amassed large, and intensity is high, the characteristic of excellent thermal conductivity.If excellent composite phase-change material prepared by graphene film and paraffin perfect adaptation to become one and challenge.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of three-dimensional phase change material based on Graphene and preparation method thereof is provided.The graphene aerogel bore hole size that the present invention obtains can regulate, thus effectively regulates the structure based on the three-dimensional phase change material of Graphene.Excellent, the applicable large-scale production and application of the composite phase-change material thermal storage performance based on graphene aerogel that this legal system is standby.
Object of the present invention is achieved through the following technical solutions: a kind of three-dimensional phase change material based on Graphene, is made up of graphene aerogel and the paraffin be filled in graphene aerogel fenestra hole, the loading level of described paraffin be 0.1 ?99.9vol%.
Based on a preparation method for the three-dimensional phase change material of Graphene, its step is as follows:
(1) be that the graphene oxide water solution of 1 ?100mg/mL enters solidification liquid after continuously and smoothly the preparation facilities with in-line die orifice extrudes by concentration, be frozen into graphene oxide gel film, graphene oxide gel film is put into liquid nitrogen quick freezing.
(2) by the graphene oxide gel film after freezing treatment under atmosphere of inert gases first with 0.1 ?1 DEG C/min ramp to 500 ?800 DEG C, be incubated 0.5 ?2h;
(3) under atmosphere of inert gases with 1 ?3 DEG C/min ramp to 1000 ?1300 DEG C, be incubated 0.5 ?3h;
(4) under atmosphere of inert gases with 5 ?8 DEG C/min ramp to 2000 ?3000 DEG C, be incubated 0.5 ?4h, obtain graphene aerogel film
(5) graphene aerogel film step 4 obtained concentration be 0.1 ?100g/ml paraffin dichloromethane solution in soak 0.5 ?10h, then to be put in 30 DEG C of vacuum drying ovens dry, to obtain the composite phase-change film based on Graphene.
Further, the mean sizes of the graphene oxide in described step 1 is greater than 50um, and distribution coefficient is 0.2 ~ 0.5.
Further, described graphene oxide gel film time of quick freezing in liquid nitrogen be set as 5 ?30min.
Beneficial effect of the present invention is:
(1) by three steps independently temperature-rise period, the functional group of graphenic surface is progressively departed from, and discharges step by step in gaseous form, meanwhile, graphitizing process stepwise development, forms the micro-air bag of Graphene; And in the forming process of micro-air bag, the most stable functional group of graphenic surface also comes off thereupon, add gas expansion under high temperature, thereby produce aerogel structure, be conducive to the filling of paraffin.
(2) the melt phase change enthalpy of the composite phase-change film based on Graphene obtained by the present invention is 175.3J/g, and solidifying enthalpy of phase change is 186.2J/g.
Embodiment
Content of the present invention is further illustrated below in conjunction with example:
Embodiment 1
(1) be that the graphene oxide water solution of 60mg/mL is placed in liquid nitrogen freezing 3min, 5min, 15min, 30min, 35min respectively by concentration.Observe under graphene oxide gel (a, b, c, d, e) after freezing treatment is placed in scanning electron microscope, graphene oxide gel a lamella is stacking more, and hole is few; Graphene oxide gel b, c, d hole is even, and compactness extent increases successively, and destroying appears in graphene oxide gel e structure.
(2) by the graphene oxide gel after freezing treatment under atmosphere of inert gases first with the ramp of 1 DEG C/min to 800 DEG C, insulation 0.5h;
(3) under atmosphere of inert gases with the ramp of 3 DEG C/min to 1300 DEG C, insulation 0.5h;
(4) under atmosphere of inert gases with the ramp of 8 DEG C/min to 3000 DEG C, insulation 0.5h, obtain graphene aerogel;
(5) by this graphene aerogel in concentration be 80g/ml paraffin dichloromethane solution in soak 3h, then to be put in 30 DEG C of vacuum drying ovens dry, obtain the composite phase-change material based on Graphene, paraffin loading level is 99.9%.By differential scanning calorimetry (DSC) test, the melt phase change enthalpy obtained based on the three-dimensional phase change material of Graphene is 156.3J/g, and solidifying enthalpy of phase change is 168.2J/g.
Embodiment 2
(1) be that the graphene oxide water solution of 1mg/mL is placed in liquid nitrogen and carries out 25min by concentration.
(2) by the graphene oxide gel after freezing treatment under atmosphere of inert gases first with the ramp of 1 DEG C/min to 800 DEG C, insulation 0.5h;
(3) under atmosphere of inert gases with the ramp of 3 DEG C/min to 1300 DEG C, insulation 0.5h;
(4) under atmosphere of inert gases with the ramp of 8 DEG C/min to 3000 DEG C, insulation 0.5h, obtain graphene aerogel;
(5) aerogel step 4 obtained is soak 5h in the dichloromethane solution of the paraffin of 10g/ml in concentration, then is put in 30 DEG C of vacuum drying ovens dry, and obtain the three-dimensional phase change material based on Graphene, paraffin loading level is 70%.By differential scanning calorimetry (DSC) test, the melt phase change enthalpy obtained based on the three-dimensional phase change material of Graphene is 126.3J/g, and solidifying enthalpy of phase change is 164.2J/g.
Embodiment 4
(1) be that the graphene oxide water solution of 100mg/mL is placed in liquid nitrogen and carries out 25min by concentration.
(2) graphene oxide gel after freezing treatment is heat-treated with the heat treatment mode shown in table 1 ~ table 3 under atmosphere of inert gases,
(3) by the aerogel after step 3 thermal treatment in concentration be 10g/ml paraffin dichloromethane solution in soak 3h, then to be put in 30 DEG C of vacuum drying ovens dry, to obtain the three-dimensional phase change material based on Graphene.
Table 1
Table 2
Table 3
As can be seen from table 1 ~ table 3, the performance of this material mainly contains two aspects and determines, one material internal graphene oxide sheet structure repair situation, i.e. the coming off and the reparation of carbon conjugated structure under high temperature of functional group.Its two, the continuity of material internal 3 D tropism structure, the i.e. connectivity of internal sheets Rotating fields.The performance of the three-dimensional phase change material of the two acting in conjunction Graphene.
In table 1, by compare A1 B1 C1 D1 the temperature of E1, A1 too low, be not enough to remove the functional group of the easy degraded of major part, cause gas in second step pyroprocess to produce fast in a large number, at high temperature tearing sheet Rotating fields; E1 temperature is too high, produces gas too fast, can tear material internal structure in a large number, both can make deterioration in material properties.Have only at B1, C1, D1 temperature, functional group can slowly and thoroughly remove, to ensure material property.By compare C1 F1 G1 H1, F1 temperature rise rate too low, air release is too slow, and material internal can not be made to form through hole; H1 temperature-rise period is too fast, and air release is too fast, tears material internal structure, is unfavorable for forming transmission path.C1 I1 J1 K1 L1 M1, I1 soaking time too short, the degraded of most of functional group can not be ensured; M1 insulating process is long, can absorb the tar inside stove, is unfavorable for the lifting of performance.J1, K1, L1 just in time avoid above both.
In table 2, by compare A2 B2 C2 D2 E2, A2 temperature rise rate too low, have a strong impact on heat conductivility.E heat-up rate is too high, can tear Graphene interlayer structure, makes the degradation of graphene aerogel.Under having the heat-up rate of B2, C2, D2 only, just can the capable thermal conductivity not only having ensured aerogel structure but also ensured Graphene.By compare C2 F2 G2 H2, F2 temperature too low, stable functional group can not fully be departed from, and in follow-up graphited process, easy transition release gas, destroys the internal structure of aerogel; By compare C2 I2 J2 K2 L2 M2, I2 soaking time too short, stable functional group can not fully come off; M2 overlong time, the easy tar adsorption of graphene aerogel, is unfavorable for the lifting of graphene aerogel performance; And under C2, J2, K2 condition, both can ensure fully coming off of stabilising functional group, the puzzlement of tar can be avoided again.
In table 3, by compare A3 B3 C3 D3 E3, A3 temperature rise rate too low, it is excessively slow that most stabilising functional group comes off, and is unfavorable for the formation of graphene aerogel conjugate network; E3 temperature-rise period is too fast, air release and high-temperature expansion too fast, easily destroy the structure of graphene aerogel.When only having B3, C3, D3, the formation that the graphene aerogel of conductive network could be stable, the structure on Graphene could be repaired slowly.By compare C3 F3 G3 H3 I3, F3 terminal temperature too low, graphene aerogel structure repair is perfect not, so various performance is all very poor; Both could ensure the reparation of graphene-structured at the temperature of C3, G3, H3, can not be destroyed again.By compare C3 J3 K3 L3 M3, J3 soaking time too low, graphene aerogel structure can not fully be repaired, and M3 soaking time is long, also can make to adsorb the tar in body of heater, affect the performance of Graphene three-dimensional phase change material.
Claims (4)
1. based on a three-dimensional phase change material for Graphene, it is characterized in that, be made up of three-dimensional grapheme aerogel and the paraffin be filled in graphene aerogel hole, the loading level of described paraffin is 0.1 ?99.9vol%.
2. based on a preparation method for the three-dimensional phase transformation of Graphene, it is characterized in that, its step is as follows:
(1) by concentration be 1 ?the graphene oxide water solution of 100mg/mL put into liquid nitrogen quick freezing.
(2) by the graphene oxide gel film after freezing treatment under atmosphere of inert gases first with 0.1 ?1 DEG C/min ramp to 500 ?800 DEG C, be incubated 0.5 ?2h;
(3) under atmosphere of inert gases with 1 ?3 DEG C/min ramp to 1000 ?1300 DEG C, be incubated 0.5 ?3h;
(4) under atmosphere of inert gases with 5 ?8 DEG C/min ramp to 2000 ?3000 DEG C, be incubated 0.5 ?4h, obtain graphene aerogel
(5) graphene aerogel step 4 obtained concentration be 0.1 ?100g/ml paraffin dichloromethane solution in soak 0.5 ?10h, then to be put in 30 DEG C of vacuum drying ovens dry, to obtain the three-dimensional phase transformation based on Graphene.
3. a kind of three-dimensional phase change material based on Graphene and preparation method thereof as claimed in claim 2, it is characterized in that, the mean sizes of the graphene oxide in described step 1 is greater than 50um, and distribution coefficient is 0.2 ~ 0.5.
4. a kind of three-dimensional phase change material based on Graphene and preparation method thereof as claimed in claim 2, is characterized in that, described graphene oxide gel film time of quick freezing in liquid nitrogen be set as 2 ?30min.
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| CN106085367A (en) * | 2016-06-17 | 2016-11-09 | 航天材料及工艺研究所 | A kind of flexible fixed phase change heat-barrier material and preparation method thereof |
| CN106602062A (en) * | 2016-12-08 | 2017-04-26 | 浙江大学 | Preparation method of graphene aerogel positive electrode material and application of graphene aerogel positive electrode material in aluminum ion battery |
| CN106634855A (en) * | 2016-10-28 | 2017-05-10 | 同济大学 | Preparation method of hybrid graphene gel/phase-change heat-conducting composite material |
| CN107674652A (en) * | 2017-08-31 | 2018-02-09 | 北京化工大学 | A kind of arbitrary shape three-dimensional grapheme thermal-conductivity phase-change composite and preparation method thereof |
| CN108997979A (en) * | 2018-07-09 | 2018-12-14 | 西南交通大学 | A kind of compound paraffin phase change material and preparation method thereof |
| CN110205100A (en) * | 2019-05-16 | 2019-09-06 | 同济大学 | Graphene oxide/expanded graphite aeroge phase change composite material and preparation method thereof |
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| CN106634855A (en) * | 2016-10-28 | 2017-05-10 | 同济大学 | Preparation method of hybrid graphene gel/phase-change heat-conducting composite material |
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| CN110564374B (en) * | 2019-09-18 | 2021-08-03 | 青海大学 | Graphene aerogel or carbon nano-particle phase change material and preparation method thereof |
| CN110564374A (en) * | 2019-09-18 | 2019-12-13 | 青海大学 | Graphene aerogel or carbon nano-particle phase change material and preparation method thereof |
| CN113698915A (en) * | 2020-05-22 | 2021-11-26 | 中国科学院大连化学物理研究所 | Graphene-based multi-response shaped composite phase change material and preparation and application thereof |
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| CN115305059A (en) * | 2022-01-28 | 2022-11-08 | 兰州理工大学 | Preparation method and application of hexadecylamine three-dimensional graphene composite material |
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