CN113045884B - Carbon fiber polyethylene glycol phase change composite material - Google Patents
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- CN113045884B CN113045884B CN202110295214.6A CN202110295214A CN113045884B CN 113045884 B CN113045884 B CN 113045884B CN 202110295214 A CN202110295214 A CN 202110295214A CN 113045884 B CN113045884 B CN 113045884B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/16—Halogen-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C08K7/04—Fibres or whiskers inorganic
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/14—Thermal energy storage
Abstract
The invention relates to a carbon fiber polyethylene glycol phase change composite material, which comprises 100 parts by weight of polyethylene glycol, 20-100 parts by weight of calcium chloride, 20-100 parts by weight of carbon fiber felt and 0.5-3 parts by weight of coupling agent; the polyethylene glycol and the calcium chloride can form a complex system, so that the problem of melting deformation of the phase-change material can be solved to a certain extent; the surface treatment of the carbon fiber felt can improve the interface combination problem of the carbon fibers and the phase change material and improve a heat conduction path.
Description
Technical Field
The invention relates to the technical field of polymer heat-conducting phase-change composite materials, in particular to a carbon fiber polyethylene glycol phase-change composite material with a three-dimensional net structure, a stable shape and a high heat conductivity coefficient and a preparation method thereof.
Background
The polymer phase-change material absorbs heat through melting when the temperature is high, releases heat through recrystallization when the ambient temperature is reduced, and keeps the temperature of the phase-change material within a certain range (melting point) in the process of heat absorption or heat release, thereby ensuring the temperature stability of the ambient environment. The characteristic that the high molecular phase change material enables the ambient temperature to be stabilized in a certain temperature range enables the high molecular phase change material to be applied to the fields of electronic refrigeration, building heating/refrigeration (indoor temperature control), floor radiant heating, thermal switches, clothing and the like.
The commonly used polymer phase-change materials and the melting points thereof are Eicosane (36 ℃), octadecane (28 ℃), 1-dodecanol (22 ℃), RT-22 (25.37 ℃), octadecanol (28.91 ℃), RT27 (28.81 ℃), and the polymer phase-change materials can ensure that the environmental temperature is kept near the melting point of the phase-change materials by absorbing heat and emitting heat. However, the thermal conductivity of the polymeric phase change materials is 0.13W/(m.K) (RT 27), 0.17W/(m.K) (octagland), 0.26W/(m.K) (RT 25), 0.36W/(m.K) (Eicosan), 0.42W/(m.K) (Tetradecanol), and 0.48W/(m.K) (Capric acid). Therefore, the body thermal conductivity of the high-molecular phase change material is generally low, and when the high-molecular phase change material is applied to rapid energy storage, heat energy cannot be rapidly stored, so that the application of the high-molecular phase change material is limited. Therefore, the thermal conductivity of the high molecular phase change material needs to be improved to meet the requirement of rapid energy storage.
At present, the heat conductivity coefficient of the high-molecular phase-change material is improved mainly by adding a high-heat-conductivity filler. For example, the thermal conductivity of the polymeric phase change material is improved by adding materials such as metal materials (silver particles, copper particles, silver nanowires, copper nanowires), ceramic materials (boron nitride, aluminum oxide), carbon materials (graphite, carbon nanofibers, carbon nanotubes, carbon black, carbon fibers), and the like. The method for obtaining high heat conductivity coefficient of the high polymer material is mainly to form a high heat conductivity channel in a high polymer matrix by the filler, namely, various methods are used to form a percolation network in the high polymer material by the filler, so that the heat conductivity coefficient of the high polymer phase change material is mutated, and the high heat conductivity coefficient is obtained. However, the traditional process method generally adds a large amount of fillers by a blending method to achieve percolation so as to improve the thermal conductivity of the material. However, if the viscosity of the polymer phase-change material is increased by adding a filler to a large extent, the processing and molding are difficult, and the enthalpy (heat storage capacity) and other performances of the polymer material are reduced. Therefore, the addition amount of the filler is as small as possible so as to avoid influencing the processing performance and the comprehensive physical performance of the high-molecular phase-change material. Through various methods, the filler can form a three-dimensional network structure in the high-molecular phase-change material, so that a high-heat-conduction passage is formed, heat can be quickly transmitted on the three-dimensional network structure, and the condition that the content of the filler is low and the heat conductivity coefficient is high is achieved. The method for forming high heat conducting path in the present high molecular composite material, especially for fiber material, mainly includes freeze-drying orientation method, electroplating forming method, self-assembly forming method, template method and other methods. These methods can improve the thermal conductivity of polymer materials several times or even several tens times, and are good methods for rapidly improving the thermal conductivity, and thus they have become hot spots for recent scientists to study.
The polymer phase-change material stores energy by a melting and heat absorption method, so that the phenomena of shrinkage deformation and flow deformation are easy to occur after the polymer material is melted, which brings difficulty to the application of the phase-change material. Therefore, in order to reduce the deformation problem of the phase change material, the phase change material needs to be confined. The method for improving the deformation of the phase-change material at the present stage mainly comprises a microcapsule method, an adsorption method, a crosslinking method and the like. If the phase change material is encapsulated in a polymer shell to form microcapsules, the polymer shell can prevent the phase change material from leaking, and the method is called a microcapsule method. For example, a method of preventing the flow of the phase change material by adsorbing the phase change material using a porous material having a relatively large specific surface area is called an adsorption method. The method of using chemical crosslinking to generate crosslinking between molecular chains of the phase-change material, thereby preventing the material from deforming is called crosslinking method. Therefore, preventing the melting deformation of the phase change material has also been a hot spot of research of related scientists in recent years.
Disclosure of Invention
The invention aims to provide a carbon fiber polyethylene glycol phase change composite material with a 3D heat conduction framework structure and capable of improving melt deformation and a preparation method thereof.
In order to solve the technical problem, the carbon fiber polyethylene glycol phase change composite material provided by the invention comprises, by mass, 100 parts of polyethylene glycol, 20-100 parts of calcium chloride, 20-100 parts of carbon fiber felt and 0.5-3 parts of a coupling agent.
Further, the polyethylene glycol is polyethylene glycol with a relative molecular weight of 200-2000; the calcium chloride is chemically pure.
Further, the carbon fiber felt has a density of 0.1-0.5 g/cm 3 The lightweight carbon/carbon composite of (1), wherein the carbon fiber content is 90%, the binder carbon content is 10%, the carbon fiber mat has an x-y-z three-dimensional network structure, the carbon fibers have a length of 10-15 cm and are isotropic in the x-y plane, the z-direction fibers have a fiber density in the x-y plane of about 1: (50-250).
Further, the coupling agent is a silane coupling agent KH550.
A preparation method of a carbon fiber polyethylene glycol phase change composite material comprises the following steps,
preparing a complexing solution in the step (a): after polyethylene glycol and calcium chloride are proportioned, putting the mixture into ethanol for dissolving for later use;
step (b) surface treatment of the carbon fiber felt: firstly, putting a carbon fiber felt into a concentrated sulfuric acid solution, soaking for 2 hours at 80 ℃, removing impurities, carrying out oxidation treatment on the surface, taking out and drying, putting the carbon fiber felt into an ethanol solution containing a silane coupling agent, carrying out reflux treatment for 8 hours at 80 ℃, taking out and drying for later use;
step (c), soaking the carbon fiber felt in a complexing solution: dipping the treated carbon fiber felt into a solution of polyethylene glycol and calcium chloride, and adsorbing the solution of polyethylene glycol and calcium chloride on the surface of the carbon fiber felt, wherein a large amount of polyethylene glycol and calcium chloride composite systems can be adsorbed and grafted through the large specific surface area of the carbon fiber felt;
step (d) drying and complex crosslinking of the complex system: putting the impregnated carbon fiber felt into an oven, drying for 24 hours at the temperature of 80 ℃, and then curing for 2 hours at the temperature of 120 ℃ to complex and crosslink polyethylene glycol and calcium chloride, wherein the aim of the step is to enable a complex system to be tightly combined to the surface of the carbon fiber felt;
step (e) repeated impregnation and complex crosslinking: repeating the steps (c) and (d) repeatedly to complex a certain amount of phase-change material composite system on the surface of the carbon fiber felt;
step (f), compression and confinement molding: the content of the phase-change material can be adjusted by adjusting the compression multiple, namely, the carbon fiber polyethylene glycol composite system subjected to complexing and crosslinking is placed into a pressing die, is cured for 2 hours at the temperature of 120 ℃ under the action of 10MPa, and is demoulded, so that the carbon fiber polyethylene glycol phase-change composite material with a three-dimensional network structure, a stable shape and a high heat conductivity coefficient is finally prepared.
The invention has the technical effects that: (1) Compared with the prior art, the carbon fiber polyethylene glycol phase change composite material disclosed by the invention has the advantages that (1) polyethylene glycol and calcium chloride can form a complex system, so that the problem of melting deformation of the phase change material can be solved to a certain extent; (2) The surface treatment of the carbon fiber felt can improve the interface combination problem of the carbon fibers and the phase change material and improve a heat conduction path; (3) The carbon fiber felt can adsorb the phase-change material and has a three-dimensional skeleton structure, so that the problem of melting deformation of the phase-change material is further solved, and meanwhile, a high-heat-conductivity passage of the carbon fiber felt can ensure that the composite material has a high heat conductivity coefficient; (4) By the high-temperature compression limited-area pressing method, pores in a composite material system can be reduced, the bonding tightness of the carbon fiber and the polyethylene glycol system is increased, a heat conduction path is improved, and finally the carbon fiber/polyethylene glycol phase-change composite material with a three-dimensional network structure, a stable shape and a high heat conductivity coefficient is prepared.
Drawings
The invention is described in further detail below with reference to the drawings:
FIG. 1 is a schematic metallographic view of a carbon fiber polyethylene glycol phase change material prepared by subjecting a carbon fiber felt to surface treatment in example 1;
FIG. 2 is a metallographic representation of a carbon fiber polyethylene glycol phase change material prepared by subjecting the carbon fiber felt to no surface treatment in example 1;
FIG. 3 is a leakage test chart of the carbon fiber polyethylene glycol phase change material under a high temperature condition.
Detailed Description
Example 1
The carbon fiber polyethylene glycol phase change composite material is prepared by the following method:
step (a), mixing polyethylene glycol (PEG 1500) and calcium chloride in a mass ratio of 5:1, adding the mixture into ethanol for dissolving for later use after proportioning;
step (b), adding carbon fiber felt (0.2 g/cm) 3 ) Soaking in concentrated sulfuric acid solution at 80 deg.C for 2 hr to remove impurities, oxidizing the surface, drying, adding into ethanol solution containing silane coupling agent, refluxing at 80 deg.C for 8 hr, and drying;
step (c), dipping the treated carbon fiber felt into a solution of polyethylene glycol and calcium chloride, and adsorbing the solution of polyethylene glycol and calcium chloride on the surface of the carbon fiber felt;
putting the impregnated carbon fiber felt into an oven, drying for 24 hours at the temperature of 80 ℃, and then curing for 2 hours at the temperature of 120 ℃ to complex and crosslink the polyethylene glycol and the calcium chloride;
repeating the steps (c) and (d) repeatedly to complex a certain amount of phase-change material composite system on the surface of the carbon fiber felt;
and (f) placing the complex crosslinked carbon fiber/polyethylene glycol composite system into a pressing mold, and curing for 2 hours at the temperature of 120 ℃ under the action of 10MPa, wherein the compression ratio is 3: and 1, demolding, and finally preparing the carbon fiber/polyethylene glycol phase change composite material with a three-dimensional network structure, a stable shape and a high heat conductivity coefficient.
The structure of the carbon fiber polyethylene glycol phase change material with a 3D network structure is shown in fig. 1 (the carbon fiber felt is subjected to surface treatment), and fig. 2 is a carbon fiber polyethylene glycol phase change material formed when the carbon fiber felt is not subjected to surface treatment. As can be seen from FIG. 1, the surface-treated carbon fiber is tightly bonded with polyethylene glycol, so as to ensure high thermal conductivity, and the polyethylene glycol can be firmly confined between the fibers to prevent deformation of the material. As can be seen from fig. 2, when the carbon fiber felt does not pass through the surface, the carbon fibers and the polyethylene glycol are loosely bonded, so that a large number of pores exist, which is not favorable for forming a high thermal conductivity path, and the thermal conductivity of the composite material can be seriously reduced. FIG. 3 is a leakage test chart of the carbon fiber polyethylene glycol phase change material under a high temperature condition. As can be seen from fig. 3, after 15min at a temperature of 80 ℃, the polyethylene glycol had undergone leakage deformation, while the polyethylene glycol/calcium chloride had slightly leaked but had no deformation, and after the carbon/carbon fiber felt was compounded, the polyethylene glycol/calcium chloride + carbon/carbon fiber felt had no leakage deformation at all, regardless of whether it was a low-content carbon fiber felt (low) or a high-content carbon fiber felt (high). The melting point, the melting enthalpy and the heat conductivity coefficient of the finally prepared phase-change material can reach 40 ℃, 95J/g and 3.2W/(mK), and the phase-change material is not easy to leak and denature.
Example 2
The carbon fiber polyethylene glycol phase change composite material is prepared by the following method:
step (a), mixing polyethylene glycol (PEG 2000) and calcium chloride in a mass ratio of 4:1, adding the mixture into ethanol for dissolving for later use;
step (b), adding carbon fiber felt (0.2 g/cm) 3 ) Soaking in concentrated sulfuric acid solution at 80 deg.C for 2 hr to remove impurities, oxidizing the surface, drying, adding into ethanol solution containing silane coupling agent, refluxing at 80 deg.C for 8 hr, and drying;
step (c), dipping the treated carbon fiber felt into a solution of polyethylene glycol and calcium chloride, and adsorbing the solution of polyethylene glycol and calcium chloride on the surface of the carbon fiber felt;
step (d), putting the impregnated carbon fiber felt into an oven, drying for 24 hours at the temperature of 80 ℃, and then curing for 2 hours at the temperature of 120 ℃ to complex and crosslink the polyethylene glycol and the calcium chloride;
repeating the steps (c) and (d) repeatedly to complex a certain amount of phase-change material composite system on the surface of the carbon fiber felt;
and (f) placing the complex crosslinked carbon fiber/polyethylene glycol composite system into a pressing mold, and curing for 2 hours at 120 ℃ under the action of 10MPa, wherein the compression ratio is 2: and 1, demolding, and finally preparing the carbon fiber/polyethylene glycol phase change composite material with a three-dimensional network structure, a stable shape and a high heat conductivity coefficient. The melting point, the melting enthalpy and the heat conductivity coefficient of the finally prepared phase-change material can reach 41 ℃, 80J/g and 2.5W/(mK), and the phase-change material is not easy to denature.
Example 3
The carbon fiber polyethylene glycol phase change composite material is prepared by the following method:
step (a), mixing polyethylene glycol (PEG 800) and calcium chloride in a mass ratio of 4:1, adding the mixture into ethanol for dissolving for later use after proportioning;
step (b), carbon fiber felt (0.2 g/cm) 3 ) Soaking in concentrated sulfuric acid solution at 80 deg.C for 2 hr to remove impurities, oxidizing the surface, drying, adding into ethanol solution containing silane coupling agent, refluxing at 80 deg.C for 8 hr, and drying;
step (c), dipping the treated carbon fiber felt into a solution of polyethylene glycol and calcium chloride, and adsorbing the solution of polyethylene glycol and calcium chloride on the surface of the carbon fiber felt;
step (d), putting the impregnated carbon fiber felt into an oven, drying for 24 hours at the temperature of 80 ℃, and then curing for 2 hours at the temperature of 120 ℃ to complex and crosslink the polyethylene glycol and the calcium chloride;
repeating the steps (c) and (d) repeatedly to complex a certain amount of phase-change material composite system on the surface of the carbon fiber felt;
and (f) placing the complex crosslinked carbon fiber/polyethylene glycol composite system into a pressing mold, and curing for 2 hours at 120 ℃ under the action of 10MPa, wherein the compression ratio is 1.5: and 1, demolding to finally prepare the carbon fiber/polyethylene glycol phase change composite material with a three-dimensional net structure, a stable shape and a high heat conductivity coefficient. The melting point, the melting enthalpy and the heat conductivity coefficient of the finally prepared phase-change material can reach 38 ℃, 78J/g and 1.5W/(mK), and the phase-change material is not easy to denature.
It should be understood that the above examples are only for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And such obvious changes and modifications as fall within the spirit of the invention are deemed to be within the scope of the invention.
Claims (4)
1. The carbon fiber polyethylene glycol phase change composite material is characterized by comprising the following components, by mass, 100 parts of polyethylene glycol, 20-100 parts of calcium chloride, 20-100 parts of carbon fiber felt and 0.5-3 parts of silane coupling agent;
the preparation method of the carbon fiber polyethylene glycol phase change composite material comprises the following steps,
preparing a complexing solution in the step (a): after polyethylene glycol and calcium chloride are proportioned, the mixture is put into ethanol for dissolving for standby;
step (b) surface treatment of the carbon fiber felt: firstly, putting a carbon fiber felt into a concentrated sulfuric acid solution, soaking for 2 hours at 80 ℃, removing impurities, carrying out oxidation treatment on the surface, taking out and drying, putting the carbon fiber felt into an ethanol solution containing a silane coupling agent, carrying out reflux treatment for 8 hours at 80 ℃, taking out and drying for later use;
step (c), soaking the carbon fiber felt in a complexing solution: dipping the treated carbon fiber felt into a solution of polyethylene glycol and calcium chloride, and adsorbing the solution of polyethylene glycol and calcium chloride on the surface of the carbon fiber felt, wherein a large amount of polyethylene glycol and calcium chloride composite systems can be adsorbed and grafted through the large specific surface area of the carbon fiber felt;
step (d) drying and complex crosslinking of the complex system: putting the impregnated carbon fiber felt into an oven, drying the carbon fiber felt for 24 hours at the temperature of 80 ℃, and then curing the carbon fiber felt for 2 hours at the temperature of 120 ℃ to complex and crosslink polyethylene glycol and calcium chloride, wherein the aim of the step is to enable a complex system to be tightly combined on the surface of the carbon fiber felt;
step (e) repeated impregnation and complex crosslinking: repeating the steps (c) and (d) repeatedly to complex a certain amount of phase-change material composite system on the surface of the carbon fiber felt;
step (f), compression and limited area molding: the content of the phase-change material can be adjusted by adjusting the compression multiple, namely, the carbon fiber polyethylene glycol composite system subjected to complexing and crosslinking is placed into a pressing die, is cured for 2 hours at the temperature of 120 ℃ under the action of 10MPa, and is demoulded, so that the carbon fiber polyethylene glycol phase-change composite material with a three-dimensional network structure, a stable shape and a high heat conductivity coefficient is finally prepared.
2. The carbon fiber polyethylene glycol phase change composite material as claimed in claim 1, wherein the polyethylene glycol is polyethylene glycol having a relative molecular weight of 200-2000; the calcium chloride is chemically pure.
3. The carbon fiber polyethylene glycol phase change composite material as claimed in claim 2, wherein the carbon fiber felt has a density of 0.1-0.5 g/cm 3 The light carbon/carbon composite material comprises 90% of carbon fibers, 10% of bonding carbon, an x-y-z three-dimensional net structure of the carbon fiber felt, 10-15 cm of the carbon fibers, isotropy in an x-y plane, and 1: (50-250).
4. The carbon fiber polyethylene glycol phase change composite material according to claim 3, wherein the silane coupling agent is silane coupling agent KH550.
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| CN202211186303.8A CN115678244A (en) | 2021-03-19 | 2021-03-19 | Preparation method of carbon fiber polyethylene glycol phase-change composite material |
| CN202211185948.XA CN115403915A (en) | 2021-03-19 | 2021-03-19 | Carbon fiber polyethylene glycol phase change composite material with 3D heat conduction skeleton structure |
| CN202110295214.6A CN113045884B (en) | 2021-03-19 | 2021-03-19 | Carbon fiber polyethylene glycol phase change composite material |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4851291A (en) * | 1986-06-19 | 1989-07-25 | The United States Of America As Represented By The Secretary Of Agriculture | Temperature adaptable textile fibers and method of preparing same |
| CN1602372A (en) * | 2001-09-21 | 2005-03-30 | 奥特拉斯技术有限公司 | Multi-component fibers having reversible thermal properties and methods of manufacturing thereof |
| CN108048045A (en) * | 2017-11-28 | 2018-05-18 | 大连理工大学 | A kind of enhanced thermal conduction organic composite shaping phase-change material and preparation method thereof |
| CN110872490A (en) * | 2019-12-10 | 2020-03-10 | 北京科技大学 | Medium-low temperature tubular carbon fiber composite phase change material and preparation method thereof |
| CN111663335A (en) * | 2020-06-17 | 2020-09-15 | 苏州科技大学 | Preparation method of flexible optical/electric-thermal double-response phase change fabric |
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| US10005941B2 (en) * | 2013-12-17 | 2018-06-26 | All Cell Technologies, Llc | Flexible phase change material composite for thermal management systems |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4851291A (en) * | 1986-06-19 | 1989-07-25 | The United States Of America As Represented By The Secretary Of Agriculture | Temperature adaptable textile fibers and method of preparing same |
| CN1602372A (en) * | 2001-09-21 | 2005-03-30 | 奥特拉斯技术有限公司 | Multi-component fibers having reversible thermal properties and methods of manufacturing thereof |
| CN108048045A (en) * | 2017-11-28 | 2018-05-18 | 大连理工大学 | A kind of enhanced thermal conduction organic composite shaping phase-change material and preparation method thereof |
| CN110872490A (en) * | 2019-12-10 | 2020-03-10 | 北京科技大学 | Medium-low temperature tubular carbon fiber composite phase change material and preparation method thereof |
| CN111663335A (en) * | 2020-06-17 | 2020-09-15 | 苏州科技大学 | Preparation method of flexible optical/electric-thermal double-response phase change fabric |
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