CN108342187A - The high heat conduction graphene aerogel composite phase-change material and preparation method of controlled shape - Google Patents
The high heat conduction graphene aerogel composite phase-change material and preparation method of controlled shape Download PDFInfo
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- CN108342187A CN108342187A CN201810121219.5A CN201810121219A CN108342187A CN 108342187 A CN108342187 A CN 108342187A CN 201810121219 A CN201810121219 A CN 201810121219A CN 108342187 A CN108342187 A CN 108342187A
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
Abstract
The present invention discloses a kind of the high heat conduction graphene aerogel composite phase-change material and preparation method of controlled shape, which includes graphene aerogel, graphene and organic phase change material.The graphene aerogel of the controlled shape is made by ethylenediamine and gelatine reduction graphite oxide, and in mass ratio 49~99：1 mixes organic phase change material with graphene, and in mass ratio 9~19:1 mixes organic phase change material with graphene aerogel, and graphene aerogel composite phase-change material is obtained by physisorphtion.The feature of graphene aerogel composite phase-change material maximum prepared by the present invention is the graphene aerogel of various shapes can be prepared according to different grinding tools, and the aeroge has high heat conduction, low supercooling, prepares the advantages such as convenient, mechanical property is good.The problems such as capable of solving the problems, such as that conventional graphite alkene aeroge composite phase-change material shape is single, and being effectively improved the high poor heat conductivity of organic phase change energy storage material, degree of supercooling, leakage.
Description
Technical field
The present invention relates to a kind of preparation methods of the high heat conduction graphene aerogel composite phase-change material of controlled shape, belong to
In phase-changing energy storage material field.
Background technology
Recently as expanding economy, demand for energy gradually increases, and non-regeneration energy consumption increases year by year,
So that energy crisis gradually aggravates.And along with the burning of fossil fuel, greenhouse gas emissions increase year by year, right
The weather in the whole world produces influence, and it is more and more urgent to increase the demand developed and used to clean reproducible energy.
Common regenerative resource such as solar energy, wind energy etc. are all periodic, at night or calm can not be received
Collection, therefore the exploitation of energy storage material is particularly important.Organic phase change material can be absorbed during phase transformation or
The a large amount of heat of release, has good thermal storage performance, is to solve energy supply and demand to distribute unbalanced lance over time and space
Shield, the effective means for improving energy utilization rate.However it is let out in organic phase change material there are thermal coefficients low, phase transition process
The problems such as dew.It solves the problems, such as that this key is exactly to be packaged to phase-change material, utilizes porous material absorption organic phase change material
It is most common means.Porous composite phase-change material preparation process is simple, and the capillary force of porous material can limit phase transformation material
Material is revealed in melting process, and the porous material with high heat conduction can improve the thermal coefficient of phase-change material.
Graphene is a kind of new material of two-dimensional nanostructure, and the graphene aerogel material occurred in recent years becomes
Research hotspot.Under alkaline reducer effect, interconnects and recombinate between graphene oxide layer, provided to construct
The graphene aerogel of three-dimensional structure.Graphene aerogel has abundant hole and open pore passage structure, can be sufficient
Phase-change material is adsorbed, the thermal conductivity of phase-change material is improved, improves the thermal stability of phase-change material.
Chinese patent CN106433564A disclose graphene aerogel complex intensifying paraffin wax type phase change heat storage material and
Preparation method.Certain density graphene oxide is mixed in a certain ratio with ascorbic acid and is restored, graphene gas is made
Graphene aerogel is dispersed in the suspension of paraffin and metal powder by gel, is kept the temperature and is ultrasonically treated, and cooling obtains graphite
The paraffin wax type phase change heat storage material of alkene aeroge complex intensifying.Patent acidic reduction agent ascorbic acid reduction-oxidation graphite,
Graphene aerogel volume contraction prepared by ascorbic acid is excessive, poor mechanical property, and the graphene aerogel shape prepared is equal
To be cylindric, graphene sheet layer accumulation is serious in aeroge, causes to conduct heat in all directions uneven, in addition reproducibility mistake
Cause oxygen-containing functional group in aeroge very few by force, be not easy and phase-change material forms hydrogen bond so that aeroge and phase-change material knot and
Property is poor.In addition metal powder heat conductivility is weaker than graphene, and the bad dispersibility in paraffin, will produce heap after multiple thermal cycle
Product.
Invention content
Technical problem：It is multiple that the purpose of the present invention is just to provide for a kind of high heat conduction graphene aerogel of controlled shape
Phase-change material and preparation method are closed, this kind of composite phase-change material improves the heat conductivility of phase-change material and avoid phase transformation material
Expect leakage phenomenon during phase transition, it is most important that this kind of method makes system by adjusting the dosage of ethylenediamine and gelatin
Standby graphene aerogel controlled shape is more advantageous to the application of graphene aerogel composite phase-change material, and the controlled shape
Graphene aerogel composite phase-change material preparation method it is simple, reaction condition is mild.
Technical solution：The present invention a kind of controlled shape high heat conduction graphene aerogel composite phase-change material, include
The graphene aerogel block of machine phase-change material, graphene and controlled shape；The graphene aerogel block of the controlled shape is by second
Diamines and gelatine reduction graphite oxide are made, the matter of the graphene aerogel block of the organic phase change material and controlled shape
It is (19~9) to measure ratio：1, the organic phase change material is (49~99) with graphene mass ratio：1.
Wherein,
The organic phase change material is paraffin, capric acid or tetradecyl alchohol.
The graphene oxide system that the graphene aerogel block of the graphene, controlled shape is prepared by Hummers methods
.
The graphene aerogel block of the controlled shape is prepared using following methods：
1) graphene oxide, ethylenediamine, gelatin is soluble in water, graphene oxide and ethylenediamine, gelatin in mass ratio 1：
(1~1.5):(0.5~0.1) it mixes, carries out reduction reaction in oil bath, obtain the graphene hydrogel of controlled shape；
2) hydrogel of controlled shape obtained is freeze-dried, obtains the graphene aerogel of controlled shape.
The graphene, by the hydrogen that graphene oxide is added to 0.5~1mol/L by the concentration of 1~2mg/mL
In sodium oxide molybdena, it is made in 80 DEG C of aqueous solution reduction reaction 12h.
Described is soluble in water by graphene oxide, ethylenediamine, gelatin, graphene oxide in water a concentration of 3~
5mg/mL。
The graphene hydrogel of the controlled shape, is mixed with ethylenediamine, gelatin by graphene oxide and is placed on difference
Heating reduction is made in the mold of shape.
Reaction condition is in the oil bath：85~95 DEG C of temperature, reaction time 8-12h.
The preparation method of the high heat conduction graphene aerogel composite phase-change material of the controlled shape of the present invention is used with lower section
It is prepared by method：
1) by organic phase change material and graphene (49~99) in mass ratio：1 mixing, it is complete to be heated to organic phase change material
Eutectic mixture is carried out supersound process 0.5-1h, obtains high-heat-conducting composite phase-transition material by running down；
2) by the high-heat-conducting composite phase-transition material and molten state high-heat-conducting composite phase-transition material in mass ratio 1:
(9~19) it mixes, is directly adsorbed using the lipophile of graphene aerogel, the cooling height for obtaining controlled shape is led
Hot graphene aerogel composite phase-change material.
Advantageous effect：In the present invention, the addition of ethylenediamine and gelatin makes graphene oxide be restored under weak basic condition,
The accumulation of graphene sheet layer and volume contraction in graphene aerogel are reduced, the mechanical property of aeroge is increased, in production
Reduction reaction can be carried out in different molds according to actual needs and prepares the graphene airsetting of controlled shape, and graphene
Addition with the heat conduction of reinforcing material and can promote phase-change material to crystallize, and reduce the degree of supercooling of phase-change material.
The present invention is compound by the graphene aerogel of organic phase change material and graphene, controlled shape, by organic phase-change
The thermal conductivity of material greatly improves；The high heat conduction graphene aerogel composite phase-change material performance of controlled shape is more stablized, can
It is used for a long time, after 200 cycles, performance is stablized；It is only ball-type or cylinder, graphene with conventional graphite alkene aeroge shape
In aeroge preparation process volume contraction acutely, poor mechanical property compare, graphene aerogel prepared by the present invention without volume receive
Contracting, controlled shape is good by gelatin crosslinking mechanical property, has expanded the application field of graphene aerogel composite phase-change material.
Specific implementation mode
The high heat conduction graphene aerogel composite phase-change material of controlled shape, raw material include organic phase change material, graphene
With graphene aerogel block.The graphene aerogel of the controlled shape is made by ethylenediamine and gelatine reduction graphite oxide,
The mass ratio of the organic phase change material and graphene aerogel is 19~9：1, the organic phase change material and graphene
Mass ratio is 49~99：1.
The organic phase change material is paraffin, capric acid, tetradecyl alchohol.
The graphene oxide that the graphene, graphene aerogel are prepared by Hummers methods is made.
The graphene aerogel block of the controlled shape is prepared using following methods：
(1) by graphene oxide and ethylenediamine, gelatin in mass ratio 1：1~1.5:0.5~0.1 mixing, in oil bath into
Row reduction reaction obtains graphene hydrogel.
(2) hydrogel obtained is freeze-dried, obtains graphene aerogel block of different shapes.
The graphene passes through in the hydrogen that graphene oxide is added to 0.5~1mol/L by the concentration of 1~2mg/mL
In sodium oxide molybdena, it is made in 80 DEG C of aqueous solution reduction reaction 12h.
The graphene oxide a concentration of 3~5mg/mL in water.
The graphene aerogel of the controlled shape is mixed with ethylenediamine, gelatin by graphene oxide and is placed on difference
It is made after heating reduction in the mold of shape.
Reaction condition is in the oil bath：85~95 DEG C of temperature, time 8-12h.
The high heat conduction graphene aerogel composite phase-change material uses following preparation method
(1) by organic phase change material and graphene in mass ratio 49~99：1 mixing, it is complete to be heated to organic phase change material
Fusing, carries out supersound process 1h by eutectic mixture, obtains high-heat-conducting composite phase-transition material.
(2) by the graphene aerogel block of controlled shape and molten state high-heat-conducting composite phase-transition material in mass ratio 1:9
~19 mixing, are directly adsorbed using the lipophile of graphene aerogel, and cooling obtains high heat conduction graphene aerogel composite phase-change
Material.
The composite phase-change material being prepared is middle material for storing heat of phase change in low temperature, and latent heat of phase change is 181.7~231.1J/
G, thermal coefficient are 1.236W/mK~1.751W/mK
With reference to embodiment, the present invention is further illustrated：
Embodiment 1
Organic phase change material selects paraffin, a concentration of 1mg/mL of graphene oxide, naoh concentration when preparing graphene
For 1mol/L, graphene oxide a concentration of 3mg/mL in water, graphene and ethylenediamine, gelatin when preparing graphene aerogel
In mass ratio 1:1:0.1 mixing, reaction condition are 85 DEG C, reaction time 8h of temperature, paraffin and graphene in composite phase-change material
Mass ratio be 99：1, the mass ratio of paraffin and graphene aerogel is 19:1.
Embodiment 2
Organic phase change material selects tetradecyl alchohol, and a concentration of 2mg/mL of graphene oxide, sodium hydroxide are dense when preparing graphene
Degree is 0.5mol/L, graphene oxide a concentration of 5mg/mL in water when preparing graphene aerogel, graphene and ethylenediamine,
Gelatin in mass ratio 1:1.5:0.1 mixing, reaction condition are 95 DEG C, reaction time 12h of temperature, tetradecyl alchohol in composite phase-change material
Mass ratio with graphene is 66：1, the mass ratio of tetradecyl alchohol and graphene aerogel is 9:1.
Embodiment 3
Organic phase change material selects capric acid, a concentration of 2mg/mL of graphene oxide, naoh concentration when preparing graphene
For 1mol/L, graphene oxide a concentration of 4mg/mL in water, graphene and ethylenediamine, gelatin when preparing graphene aerogel
In mass ratio 1:1:0.5 mixing, reaction condition are 90 DEG C, reaction time 10h of temperature, capric acid and graphite in composite phase-change material
The mass ratio of alkene is 66：1, the mass ratio of capric acid and graphene aerogel is 19:1.
Embodiment 4
Organic phase change material selects paraffin, a concentration of 1mg/mL of graphene oxide, naoh concentration when preparing graphene
For 0.5mol/L, graphene oxide a concentration of 5mg/mL in water when preparing graphene aerogel is graphene and ethylenediamine, bright
Glue in mass ratio 1：1.25:0.5 mixing, reaction condition are 90 DEG C, reaction time 12h of temperature, in composite phase-change material paraffin with
The mass ratio of graphene is 49：1, the mass ratio of paraffin and graphene aerogel is 14:1.
Embodiment 5
Organic phase change material selects tetradecyl alchohol, and a concentration of 1mg/mL of graphene oxide, sodium hydroxide are dense when preparing graphene
Degree is 1mol/L, graphene oxide a concentration of 5mg/mL in water when preparing graphene aerogel, graphene and ethylenediamine, bright
Glue in mass ratio 1:1.25:0.3 mixing, reaction condition are 85 DEG C, reaction time 10h of temperature, tetradecyl alchohol in composite phase-change material
Mass ratio with graphene is 49：1, the mass ratio of tetradecyl alchohol and graphene aerogel is 9:1.
Above-described embodiment is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill of the art
For personnel, without departing from the principle of the present invention, several improvement and equivalent replacement can also be made, these are to this hair
Bright claim be improved with the technical solution after equivalent replacement, each fall within protection scope of the present invention.
Claims (9)
1. a kind of high heat conduction graphene aerogel composite phase-change material of controlled shape, it is characterised in that：The composite phase-change material
Graphene aerogel block including organic phase change material, graphene and controlled shape；The graphene aerogel of the controlled shape
Block is made by ethylenediamine and gelatine reduction graphite oxide, the graphene aerogel block of the organic phase change material and controlled shape
Mass ratio be (19~9)：1, the organic phase change material is (49~99) with graphene mass ratio：1.
2. the high heat conduction graphene aerogel composite phase-change material of controlled shape as described in claim 1, which is characterized in that institute
The organic phase change material stated is paraffin, capric acid or tetradecyl alchohol.
3. the high heat conduction graphene aerogel composite phase-change material of controlled shape as described in claim 1, which is characterized in that institute
The graphene oxide that the graphene aerogel block of the graphene, controlled shape stated is prepared by Hummers methods is made.
4. the high heat conduction graphene aerogel composite phase-change material of controlled shape according to claim 1, it is characterised in that,
The graphene aerogel block of the controlled shape is prepared using following methods：
1) graphene oxide, ethylenediamine, gelatin is soluble in water, graphene oxide and ethylenediamine, gelatin in mass ratio 1：(1~
1.5):(0.5~0.1) it mixes, carries out reduction reaction in oil bath, obtain the graphene hydrogel of controlled shape；
2) hydrogel of controlled shape obtained is freeze-dried, obtains the graphene aerogel of controlled shape.
5. the high heat conduction graphene aerogel composite phase-change material of controlled shape according to claim 1, it is characterised in that,
The graphene, by the way that graphene oxide is added to by the concentration of 1~2mg/mL in the sodium hydroxide of 0.5~1mol/L,
It is made in 80 DEG C of aqueous solution reduction reaction 12h.
6. the high heat conduction graphene aerogel composite phase-change material of controlled shape according to claim 4, it is characterised in that,
Described is soluble in water by graphene oxide, ethylenediamine, gelatin, a concentration of 3~5mg/mL of graphene oxide in water.
7. the high heat conduction graphene aerogel composite phase-change material of controlled shape according to claim 4, it is characterised in that,
The graphene hydrogel of the controlled shape, is mixed with ethylenediamine, gelatin by graphene oxide and is placed on mould of different shapes
Heating reduction is made in tool.
8. the high heat conduction graphene aerogel composite phase-change material of controlled shape according to claim 4, it is characterised in that,
Reaction condition is in the oil bath：85~95 DEG C of temperature, reaction time 8-12h.
9. a kind of preparation side of the high heat conduction graphene aerogel composite phase-change material of controlled shape as described in claim 1
Method, which is characterized in that the high heat conduction graphene aerogel composite phase-change material is prepared using following methods：
1) by organic phase change material and graphene (49~99) in mass ratio：1 mixing, it is completely molten to be heated to organic phase change material
Change, eutectic mixture is subjected to supersound process 0.5-1h, obtains high-heat-conducting composite phase-transition material；
2) by the high-heat-conducting composite phase-transition material and molten state high-heat-conducting composite phase-transition material in mass ratio 1:(9~19) it mixes
It closes, is directly adsorbed using the lipophile of graphene aerogel, the cooling high heat conduction graphene aerogel for obtaining controlled shape is compound
Phase-change material.
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Cited By (12)
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| CN109729699A (en) * | 2019-01-11 | 2019-05-07 | 厦门大学 | A kind of phase transformation graphene heat-conducting pad, preparation method and applications |
| CN109870061A (en) * | 2019-03-27 | 2019-06-11 | 山东星火科学技术研究院 | A kind of phase-change energy storage device and preparation method thereof |
| CN110452667A (en) * | 2019-08-27 | 2019-11-15 | 国科瑞华(天津)材料科技有限公司 | Graphene, which enhances phase transformation material preparation method and graphene, enhances phase-change material |
| CN110655910A (en) * | 2019-11-13 | 2020-01-07 | 南京工业大学 | Preparation method of graphene aerogel phase-change energy storage material |
| CN112724936A (en) * | 2021-01-26 | 2021-04-30 | 山西万家暖节能科技有限公司 | Preparation method of new energy storage material |
| CN112778980A (en) * | 2021-01-26 | 2021-05-11 | 山西万家暖节能科技有限公司 | Energy storage new material for improving heat transfer and mass transfer efficiency |
| CN112812750A (en) * | 2021-01-26 | 2021-05-18 | 山西万家暖节能科技有限公司 | Application of silane coupling agent in new energy storage material and new solar energy heat supply system |
| CN113265228A (en) * | 2021-04-26 | 2021-08-17 | 西南交通大学 | Multi-energy-driven shape-stabilized phase change material and preparation method thereof |
| CN113372883A (en) * | 2021-06-07 | 2021-09-10 | 山东国烯新材料创新中心有限公司 | High-thermal-conductivity composite phase change material based on solvent replacement method and preparation method thereof |
| CN113583634A (en) * | 2021-07-22 | 2021-11-02 | 南通强生石墨烯科技有限公司 | Intelligent graphene temperature-sensing phase change fiber |
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| CN114525112A (en) * | 2022-02-28 | 2022-05-24 | 重庆大学 | Improved graphene aerogel and polyethylene glycol composite phase change material and preparation method thereof |
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| CN109729699A (en) * | 2019-01-11 | 2019-05-07 | 厦门大学 | A kind of phase transformation graphene heat-conducting pad, preparation method and applications |
| CN109870061A (en) * | 2019-03-27 | 2019-06-11 | 山东星火科学技术研究院 | A kind of phase-change energy storage device and preparation method thereof |
| CN110452667A (en) * | 2019-08-27 | 2019-11-15 | 国科瑞华(天津)材料科技有限公司 | Graphene, which enhances phase transformation material preparation method and graphene, enhances phase-change material |
| CN110655910B (en) * | 2019-11-13 | 2021-06-22 | 南京工业大学 | Preparation method of graphene aerogel phase-change energy storage material |
| CN110655910A (en) * | 2019-11-13 | 2020-01-07 | 南京工业大学 | Preparation method of graphene aerogel phase-change energy storage material |
| 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 |
| CN112778980B (en) * | 2021-01-26 | 2021-12-14 | 山西万家暖节能科技有限公司 | Energy storage new material for improving heat transfer and mass transfer efficiency |
| CN112812750A (en) * | 2021-01-26 | 2021-05-18 | 山西万家暖节能科技有限公司 | Application of silane coupling agent in new energy storage material and new solar energy heat supply system |
| CN112778980A (en) * | 2021-01-26 | 2021-05-11 | 山西万家暖节能科技有限公司 | Energy storage new material for improving heat transfer and mass transfer efficiency |
| CN112724936A (en) * | 2021-01-26 | 2021-04-30 | 山西万家暖节能科技有限公司 | Preparation method of new energy storage material |
| CN112812750B (en) * | 2021-01-26 | 2021-12-14 | 山西万家暖节能科技有限公司 | Application of silane coupling agent in new energy storage material and new solar energy heat supply system |
| CN113265228A (en) * | 2021-04-26 | 2021-08-17 | 西南交通大学 | Multi-energy-driven shape-stabilized phase change material and preparation method thereof |
| CN113372883A (en) * | 2021-06-07 | 2021-09-10 | 山东国烯新材料创新中心有限公司 | High-thermal-conductivity composite phase change material based on solvent replacement method and preparation method thereof |
| CN113372883B (en) * | 2021-06-07 | 2022-05-17 | 山东国烯新材料创新中心有限公司 | High-thermal-conductivity composite phase change material based on solvent replacement method and preparation method thereof |
| CN113583634A (en) * | 2021-07-22 | 2021-11-02 | 南通强生石墨烯科技有限公司 | Intelligent graphene temperature-sensing phase change fiber |
| CN114525112A (en) * | 2022-02-28 | 2022-05-24 | 重庆大学 | Improved graphene aerogel and polyethylene glycol composite phase change material and preparation method thereof |
| CN114525112B (en) * | 2022-02-28 | 2024-01-05 | 重庆大学 | Improved graphene aerogel and polyethylene glycol composite phase change material and preparation method thereof |
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