CN109321211A - A kind of graphitization graded porous carbon composite phase-change energy storage material and preparation method thereof - Google Patents
A kind of graphitization graded porous carbon composite phase-change energy storage material and preparation method thereof Download PDFInfo
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- CN109321211A CN109321211A CN201811223926.1A CN201811223926A CN109321211A CN 109321211 A CN109321211 A CN 109321211A CN 201811223926 A CN201811223926 A CN 201811223926A CN 109321211 A CN109321211 A CN 109321211A
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- 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
- 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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Abstract
The invention discloses a kind of graphitization graded porous carbon composite phase-change energy storage materials and preparation method thereof, it is raw material that it, which is by using cheap carbon matrix precursor and graphitization catalyst, pore creating material, prepares graphitization graded porous carbon through techniques such as ball milling mixing, charings；Again using obtained graphitization graded porous carbon as backing material, carry out compound obtaining the graphitization graded porous carbon composite phase-change energy storage material with phase-change material.Porous carbon materials obtained by the present invention have the classifying porous network structure of three-dimensional intercommunication and high graphitization degree, not only contribute to the sizing encapsulation of phase-change material, while can provide good heat conduction network channel, enhance heat transfer property；And porous carbon materials are prepared using the additive of metalline, part metals substance is restored using carbothermic reduction reaction during the preparation process, to further increase the heating conduction of material, to obtain having high thermal conductivity, chemical stability good and the composite phase-change energy storage material of heat accumulation effect.
Description
Technical field
The invention belongs to carbon materials technical fields, and in particular to a kind of graphitization graded porous carbon composite phase change energy-storing material
Material and preparation method thereof.
Background technique
In the present age of industrial high speed development, the energy has become the main drive promoted the social economic development.And it is current
Energy resource structure is made it possible to still based on the non-renewable energy resources such as fossil fuel, and due to the problems such as reserves are limited and excessive exploitation
Source exhaustion and environmental pollution already become an important factor for restricting social development, for this purpose, finding the renewable of exploitation clean and effective
New energy and the utilization rate for improving the energy have become current urgent task.Phase-change material is cheap and has high-energy close
Degree can absorb in phase transition process or discharges a large amount of thermal energy, therefore can preferably solve energy shortage and energy supply and demand mismatch
The problem of, to improve the utilization rate of the energy, this becomes current research hotspot, and in air conditioner energy saving, construction material, too
The fields such as positive heat energy utilization, space flight and aviation and electronic equipment dissipating heat have wide application prospect.
Traditional phase-change material is broadly divided into inorganic phase-changing material and organic phase change material, and wherein inorganic phase-changing material has
The advantages such as thermal coefficient is high, energy storage density is big, but that there are corrosivity is big, degree of supercooling is big and is easy to the deficiencies of mutually separating；And it is organic
Though phase-change material have many advantages, such as cheap, stable chemical performance, corrosivity it is small, substantially without supercooling and phenomenon of phase separation,
It is low there are thermal coefficient and is easy to the disadvantages of revealing, this limits their direct application to a certain extent.Therefore, in order to
Overcome the shortcomings of single inorganic or organic phase change material, phase-change material is mixed in support substrate material, it is packaged
To composite phase-change energy storage material, can using the synergistic effect between them, obtain better than single phase-change material heating conduction and
Chemical stability, thus its application field of further expansion.
The main organic material of currently used encapsulating material and inorganic material, wherein inorganic material (such as montmorillonite, expansion leech
Stone, carbon material), especially three-dimensional porous carbon material has the heating conduction and thermal stability better than organic material, is drawn
Enter in phase-change material, the thermal coefficient and chemical stability of material can be substantially improved.But most three-dimensional porous carbon exists big
The macroporous structure or microcellular structure of amount, macroporous structure are poor to the adsorption effect of phase-change material, and microcellular structure is then unfavorable for phase
The molecular motion for becoming material, both reduces its latent heat of phase change, energy storage effect is poor to a certain extent.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of graphitization graded porous carbon composite phase change energy-storing materials
Material and preparation method thereof, has the characteristics that high thermal conductivity, chemical stability are good and heat accumulation effect is good, and preparation method work
Skill is simple, at low cost, environmental-friendly.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of graphitization graded porous carbon composite phase-change energy storage material, preparation method include the following steps:
(1) it is graphitized the preparation of graded porous carbon: carbon matrix precursor, graphitization catalyst and pore creating material being mixed, and mixing is added
The solvent that 1 ~ 10 times of object weight, 100r/min ~ 600r/min ball milling 0.5h~6h, is put into drying box, 60 after ball milling
~100 DEG C of dry 2 ~ 12h are placed into atmosphere furnace, in the protectiveness of nitrogen or argon gas with removing solvent after being cooled to room temperature
In atmosphere, 500 DEG C ~ 1100 DEG C are warming up to 1 DEG C/min ~ 10 DEG C/min speed, 3h ~ 6h is kept the temperature, must be graphitized classifying porous
Carbon is cooled to room temperature spare；
(2) be graphitized the preparation of graded porous carbon composite phase-change energy storage material: will graphitization graded porous carbon obtained by step (1) in
Ultrasonic disperse 1h in dehydrated alcohol adds phase-change material, and is heated on the fusing point of phase-change material, stirs 1h~3h, so
It is dry to constant weight in 80 DEG C afterwards, it takes out after being cooled to room temperature to get the graphitization graded porous carbon composite phase-change energy storage material.
The mass ratio of carbon matrix precursor used, graphitization catalyst and pore creating material is 1:(1 ~ 10 in step (1)): (1 ~ 10).
Wherein, the carbon matrix precursor be selected from coal tar pitch and petroleum asphalt, bitumen, mesophase pitch, wood pitch, lignin,
Phenolic resin, epoxy resin, bimaleimide resin, polycarbonate resin, polyimide resin, furfural resin, furfuryl alcohol resin
Any one in rouge, furane resins.
The graphitization catalyst is aluminium oxide, aluminium isopropoxide, aluminum nitrate, aluminum sulfate, aluminium chloride, aluminum acetate, hydroxide
Aluminium, sodium metaaluminate, aluminum phosphate, alumina silicate, aluminium acetate, aluminium triformate, oxalic acid aluminium, propionic acid aluminium, aluminium secondary butylate, aluminium ethylate, aluctyl,
Iron chloride, ferric nitrate, ferrous sulfate, ferrous lactate, ferric stearate, ferrous carbonate, ferric phosphate, ferric sulfate, in ironic citrate
Any one.
The pore creating material be magnesia, nano magnesia, anhydrous magnesium sulfate, magnesium acetate, magnesium stearate, basic magnesium carbonate,
Any one in magnesium citrate.
In step (1) solvent for use be water, ethyl alcohol, methylene chloride, n-butanol, isopropanol, N,N-dimethylformamide, N,
N- dimethyl acetamide, N-METHYLFORMAMIDE, ethylene glycol, any one in N-Methyl pyrrolidone.
In step (2) it is used graphitization graded porous carbon and phase-change material mass ratio be 0.1:1 ~ 3:10.Wherein, described
Phase-change material is stearic acid, paraffin, lauric acid, palmitinic acid, any one in myristic acid.
The beneficial effects of the present invention are:
(1) the multistage porous carbon materials of graphitization prepared by the present invention have hierarchical porous structure and based on mesoporous, to phase-change material
Adsorption effect it is preferable, use its for backing material be conducive to improve phase-change material latent heat and solve phase-change material in phase transformation
Leakage problem in journey, and it holds structure with high hole, is conducive to the energy storage density for improving phase change composite material.Meanwhile this is more
Grade porous carbon materials have the graphitization porous network structure of three-dimensional intercommunication, it is possible to provide good heat conduction network channel is conducive to
The transmitting of acceleration molecular enhances heat transfer property.
(2) present invention prepares porous carbon materials using the additive of metalline, restores using carbothermic reduction reaction
Part metals substance out, to further increase the heating conduction of material.
(3) compound prepared by the present invention has given full play to the synergistic effect of component, that is, improves the thermally conductive of composite material
Property be able to maintain higher latent heat of phase change again, have high thermal conductivity, chemical stability good and the advantages such as heat accumulation effect is good, and its system
It is Preparation Method simple process, at low cost, environmental-friendly, with good application prospect and economic benefit.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture of 1 step 1) of embodiment graphitization graded porous carbon obtained；
Fig. 2 is the scanning electron microscopic picture of graphitization graded porous carbon composite phase-change energy storage material prepared by embodiment 1；
Fig. 3 is the scanning electron microscopic picture of graphitization graded porous carbon composite phase-change energy storage material prepared by embodiment 2；
Fig. 4 is the scanning electron microscopic picture of graphitization graded porous carbon composite phase-change energy storage material prepared by embodiment 3；
Fig. 5 is the scanning electron microscopic picture of graphitization graded porous carbon composite phase-change energy storage material prepared by embodiment 4；
Fig. 6 is the scanning electron microscopic picture of graphitization graded porous carbon composite phase-change energy storage material prepared by embodiment 5.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
Embodiment 1
(1) 1:2:1 in mass ratio weighs phenolic resin, aluminium isopropoxide and nano magnesia respectively, and 2 times of quality of mixture are added
Ethyl alcohol, after 300r/min ball milling 3h, be put into 80 DEG C of drying boxes and keep the temperature distilling off solvent, place into gas after being cooled to room temperature
In atmosphere furnace, it is passed through nitrogen, 1100 DEG C is warming up to the speed of 5 DEG C/min, keeps the temperature 3h, obtain graphitization graded porous carbon, be cooled to
It is taken out after room temperature spare；The specific surface area of obtained graphitization graded porous carbon is 991m2/ g, Kong Rongwei 2.53cm3/ g is put down
Equal aperture is 3.2nm, Al content 0.56wt%；
(2) 0.5:9.5 in mass ratio weighs graphitization graded porous carbon and stearic acid respectively, and graphitization graded porous carbon is added to
Then ultrasound 1h in dehydrated alcohol is added stearic acid and is heated to 80 DEG C, stirring 1h is subsequently placed in 80 DEG C of vacuum oven
Drying takes out after being cooled to room temperature to constant weight and obtains graphitization graded porous carbon composite phase-change energy storage material；It is preparation-obtained
The fusing point of composite phase-change energy storage material is 66.5 DEG C, latent heat of phase change 204.7J/g, thermal conductivity 4.6W/mK.
Embodiment 2
(1) 1:1:1 in mass ratio weighs coal tar pitch, ferrous sulfate and magnesium citrate respectively, and 4 times of quality of mixture are added just
Butanol after 500r/min ball milling 2h, is put into 100 DEG C of drying boxes and keeps the temperature distilling off solvent, place into gas after being cooled to room temperature
In atmosphere furnace, it is passed through argon gas, 900 DEG C is warming up to the speed of 10 DEG C/min, keeps the temperature 4h, obtain graphitization graded porous carbon, be cooled to
It is taken out after room temperature spare；The specific surface area of obtained graphitization graded porous carbon is 759m2/ g, Kong Rongwei 1.93cm3/ g is put down
Equal aperture is 2.6 nm, and Fe content is 0.32wt%；
(2) 1:9 in mass ratio weighs graphitization graded porous carbon and paraffin respectively, and graphitization graded porous carbon is added to anhydrous second
Then ultrasound 1h in alcohol is added paraffin and is heated to 70 DEG C, stirring 1h is subsequently placed in 80 DEG C of vacuum oven and dries to perseverance
Weight takes out after being cooled to room temperature and obtains graphitization graded porous carbon composite phase-change energy storage material；Preparation-obtained composite phase-change
The fusing point of energy storage material is 54.5 DEG C, latent heat of phase change 215J/g, thermal conductivity 3.3W/mK.
Embodiment 3
(1) 1:2:3 in mass ratio weighs lignin, ferric stearate and magnesia respectively, and the dichloro of 3 times of quality of mixture is added
Methane after 450r/min ball milling 1.5h, is put into 70 DEG C of drying boxes and keeps the temperature distilling off solvent, place into gas after being cooled to room temperature
In atmosphere furnace, it is passed through nitrogen, 1000 DEG C is warming up to the speed of 8 DEG C/min, keeps the temperature 3.5h, obtain graphitization graded porous carbon, it is cooling
It is taken out after to room temperature spare；The specific surface area of obtained graphitization graded porous carbon is 599m2/ g, Kong Rongwei 2.01cm3/ g,
Average pore size is 3.3 nm, and Mg content is 0.23wt%；
(2) 1.5:8.5 in mass ratio weighs graphitization graded porous carbon and myristic acid respectively, and graphitization graded porous carbon is added
Then the ultrasound 1h into dehydrated alcohol is added myristic acid and is heated to 80 DEG C, stirring 1h is subsequently placed in 80 DEG C of vacuum drying
It is dried in case to constant weight, is taken out after being cooled to room temperature and obtain graphitization graded porous carbon composite phase-change energy storage material；Prepared
The fusing point of the composite phase-change energy storage material arrived is 65.6 DEG C, latent heat of phase change 189.7J/g, thermal conductivity 2.9W/mK.
Embodiment 4
(1) 1:1:1 in mass ratio weighs epoxy resin, aluminum sulfate and basic magnesium carbonate respectively, and 2 times of quality of mixture are added
Methylene chloride after 400r/min ball milling 2.5h, is put into 70 DEG C of drying boxes and keeps the temperature distilling off solvent, put again after being cooled to room temperature
Enter in atmosphere furnace, be passed through nitrogen, is warming up to 800 DEG C with the speed of 5 DEG C/min, keeps the temperature 4h, obtain graphitization graded porous carbon, it is cooling
It is taken out after to room temperature spare；The specific surface area of obtained graphitization graded porous carbon is 633m2/ g, Kong Rongwei 3.21cm3/ g,
Average pore size is 3.9 nm, Al content 0.19wt%；
(2) 0.5:9.5 in mass ratio weighs graphitization graded porous carbon and paraffin respectively, and graphitization graded porous carbon is added to nothing
Then ultrasound 1h in water-ethanol is added paraffin and is heated to 70 DEG C, stirring 1h is subsequently placed in 80 DEG C of vacuum oven dry
To constant weight, is taken out after being cooled to room temperature and obtain graphitization graded porous carbon composite phase-change energy storage material；It is preparation-obtained compound
The fusing point of phase-changing energy storage material is 55.1 DEG C, latent heat of phase change 233J/g, thermal conductivity 2.8W/mK.
Embodiment 5
(1) 1:3:2 in mass ratio weighs bitumen, ferric sulfate and magnesium acetate respectively, and the isopropyl of 4 times of quality of mixture is added
Alcohol after 500r/min ball milling 1.5h, is put into 90 DEG C of drying boxes and keeps the temperature distilling off solvent, place into atmosphere after being cooled to room temperature
In furnace, it is passed through nitrogen, 1050 DEG C is warming up to the speed of 4 DEG C/min, keeps the temperature 3h, obtain graphitization graded porous carbon, be cooled to room
It is taken out after temperature spare；The specific surface area of obtained graphitization graded porous carbon is 836m2/ g, Kong Rongwei 2.21cm3/ g, it is average
Aperture is 2.4 nm, and Fe content is 0.43wt%；
(2) 0.4:9.6 in mass ratio weighs graphitization graded porous carbon and myristic acid respectively, and graphitization graded porous carbon is added
Then the ultrasound 1h into dehydrated alcohol is added myristic acid and is heated to 70 DEG C, stirring 1h is subsequently placed in 80 DEG C of vacuum drying
It is dried in case to constant weight, is taken out after being cooled to room temperature and obtain graphitization graded porous carbon composite phase-change energy storage material；Prepared
The fusing point of the composite phase-change energy storage material arrived is 53.1 DEG C, latent heat of phase change 153J/g, thermal conductivity 2.3W/mK.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (10)
1. a kind of preparation method for being graphitized graded porous carbon composite phase-change energy storage material, it is characterised in that: including walking as follows
It is rapid:
(1) it is graphitized the preparation of graded porous carbon
Carbon matrix precursor, graphitization catalyst and pore creating material are mixed, and the solvent for being added 1 ~ 10 times of mixture weight carries out ball milling,
The dry removal solvent after ball milling, is cooled to after room temperature to place into and carries out carbonization reaction in atmosphere furnace, must be graphitized point
Grade porous carbon, is cooled to room temperature spare；
(2) it is graphitized the preparation of graded porous carbon composite phase-change energy storage material
It will be graphitized graded porous carbon ultrasonic disperse 1h in dehydrated alcohol obtained by step (1), adds phase-change material, and heat
To the fusing point of phase-change material, 1h ~ 3h is stirred, it is then dry to constant weight in 80 DEG C, it takes out after being cooled to room temperature to get described
It is graphitized graded porous carbon composite phase-change energy storage material.
2. preparation method according to claim 1, it is characterised in that: carbon matrix precursor used, graphitization catalysis in step (1)
The mass ratio of agent and pore creating material is 1:(1 ~ 10): (1 ~ 10).
3. preparation method according to claim 1 or 2, it is characterised in that: the carbon matrix precursor is coal tar pitch, petroleum drip
Blueness, bitumen, mesophase pitch, wood pitch, lignin, phenolic resin, epoxy resin, bimaleimide resin, poly- carbon
Acid ester resin, polyimide resin, furfural resin, furfuryl alcohol resin, any one in furane resins.
4. preparation method according to claim 1 or 2, it is characterised in that: the graphitization catalyst is aluminium oxide, isopropyl
Aluminium alcoholates, aluminum nitrate, aluminum sulfate, aluminium chloride, aluminum acetate, aluminium hydroxide, sodium metaaluminate, aluminum phosphate, alumina silicate, aluminium acetate, formic acid
Aluminium, oxalic acid aluminium, propionic acid aluminium, aluminium secondary butylate, aluminium ethylate, aluctyl, iron chloride, ferric nitrate, ferrous sulfate, ferrous lactate, tristearin
Sour iron, ferrous carbonate, ferric phosphate, ferric sulfate, any one in ironic citrate.
5. preparation method according to claim 1 or 2, it is characterised in that: the pore creating material is magnesia, nano oxidized
Magnesium, anhydrous magnesium sulfate, magnesium acetate, magnesium stearate, basic magnesium carbonate, any one in magnesium citrate.
6. preparation method according to claim 1, it is characterised in that: solvent for use is water, ethyl alcohol, dichloro in step (1)
Methane, n-butanol, isopropanol, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-METHYLFORMAMIDE, ethylene glycol, N- first
Any one in base pyrrolidones.
7. preparation method according to claim 1, it is characterised in that: in step (1) revolving speed of ball milling be 100r/min ~
600r/min, time are 0.5h~6h；Carbonization reaction is carried out in the protective atmosphere of nitrogen or argon gas, and heating rate is
1 DEG C/min ~ 10 DEG C/min, reaction temperature is 500 DEG C ~ 1100 DEG C, and the time is 3h ~ 6h.
8. preparation method according to claim 1, it is characterised in that: in step (2) graphitization graded porous carbon used and
The mass ratio of phase-change material is 0.1:1 ~ 3:10.
9. preparation method according to claim 1 or 8, it is characterised in that: the phase-change material is stearic acid, paraffin, the moon
Cinnamic acid, palmitinic acid, any one in myristic acid.
10. one kind is graphitized graded porous carbon composite phase-change energy storage material as made from any one of claim 1 ~ 9.
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