CN102605463A - Preparation method and application for fatty acid/polymer shaped phase-change superfine complex fiber - Google Patents
Preparation method and application for fatty acid/polymer shaped phase-change superfine complex fiber Download PDFInfo
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Abstract
The invention relates to a fatty acid/polymer phase-change energy-storing superfine complex fiber and a preparation method thereof and belongs to the technical field of overlapping a fiber material, a phase-change energy-storing material and a nanometer compound material. The invention specifically relates to a preparation for a binary fatty acid eutectic mixture and shaped phase-change energy-storing superfine complex fiber. The binary fatty acid/polymer phase-change energy-storing superfine complex fiber has lower phase-change temperature and higher phase-change latent heat. Meanwhile, according to the category of the selected long-chain fatty acid and difference in mixing proportion, the phase-change temperature and the phase-change latent heat of the binary fatty acid mixture are regulated and controlled, so that the phase-change temperature and the phase-change latent heat of the prepared phase-change energy-storing superfine complex fiber are different. The solid state of the superfine complex fiber before and after being subjected to phase change is kept; the phenomena, such as phase separating and the like, are avoided; and the complex fiber is widely applied to various fields, such as indoor and decorative non-woven, building energy-saving material, biological or medical material, phase-change energy-storing air-conditioning system, heat-storing temperature-adjusting fiber, functional textile, and the like.
Description
Technical field
The invention belongs to fibrous material, phase-changing energy storage material and nano composite material technology crossing domain; The method that is specifically related to adopt melting mixing and sonic oscillation to combine prepares binary aliphatic acid, and to utilize high-voltage electrostatic spinning preparation be the method for backing material, the regulatable fixed phase change superfine composite fiber of phase transition temperature with the polymer superfine fibre.
Background technology
Phase-change accumulation energy is the importance of utilization of new energy resources and Study on energy saving, and the phase transition process of phase-change material is an isothermal or approximate constant temperature process, with this temperature of coming the hierarchy of control or environment, has the function of thermal energy storage and temperature adjusting.Phase-changing energy storage material has advantages such as storage density is big, the heat vessel volume is little, the thermal efficiency is high, the suction exothermic temperature is constant.In phase-changing energy storage material; Aliphatic acid is one type of organic type of phase-change material commonly used; Have that latent heat of phase change is big, solid forming property better, is not prone to surfusion and be separated, advantage such as good heat endurance and chemical stability, nontoxic, non-corrosiveness and low price and enjoy people to pay close attention to.Yet the phase transition temperature of single fat acid is higher, is difficult to adapt to actual weather requirement, and this has limited their application in reality.Can its latent heat of phase change (or temperature) be carried out suitable adjusting through preparation binary aliphatic acid eutectic, enlarge its suitable application area in reality.At present, the aliphatic acid eutectic has been considered to the phase-change material of one type of excellent performance.But; Seepage appears in the aliphatic acid of fusion easily in practical application; Therefore adopt canister splendid attire or microcapsules that it is encapsulated usually; Though solved the leakage problems that solid-liquid phase change brings like this, the container that is made into different shape with metal material has not only hindered the heat transmission of phase-change material but also has increased cost; Though microencapsulated phase change material brings great convenience to application in addition, the encapsulation ratio of material is lower, greatly reduces the heat storage capacity of microcapsules.Therefore a kind of research of novel shaping phase-change material has received widely to be paid close attention to.
Shaping phase-change material is one type of composite phase-change material in fact, and main constituent has two kinds: (1) phase-change material, utilize its solid-liquid phase change to carry out energy storage; (2) backing material, its effect are nonflowing character and the machinabilitys that keeps composite, and the fusing point of backing material is generally higher, the stable shape and the material property that also can keep its solid of physical and chemical performance in the phase transformation range of phase-change material.Be about to low-melting phase-change material and be dispersed among the higher backing material of fusing point, as long as running temperature is not higher than the temperature that backing material can bear, this composite can maintain solid state.Shaping phase-change material not only can make material when phase transformation, keep macroshape not change, and has solved leakage problems; But also can improve the encapsulation ratio of phase-change material, be a kind of extremely promising composite phase-change material.
Electrostatic spinning is a kind of important technology of preparation micron order or nano level superfine polymer fiber.Polymer fiber through the electrostatic spinning preparation has the advantages such as network configuration that specific area is big, porosity is high and unique, can be widely used in fields such as filtering material, protective clothing, biomedicine, sensor and solar cell.People such as the Chen Yan of Donghua University mould have reported a kind of phase transformation composite spinning stoste and preparation and application in publication number is the patent of CN1493720A.Guangzhou Inst of Chemistry, Chinese Academy of Sciences's fourth grace bravely waits the people in publication number is the patent of CN 1916248A, to report a kind of super fine composite terylene fibers storing energy through phase change and preparation method thereof.But the research that utilizes electrospinning process to prepare binary aliphatic acid/polymer fixed phase change superfine composite fiber does not appear in the newspapers as yet.
Summary of the invention
In order to overcome in single fat acid phase transition temperature height and the practical application shortcomings such as temperature applicable range is narrow, the object of the present invention is to provide that a kind of latent heat of phase change and phase transition temperature are adjustable, the fixed phase change superfine composite fiber of Heat stability is good, phase transition process ne-leakage.
Another object of the present invention be to provide a kind of above-mentioned fixed phase change superfine composite fiber the preparation method and indoor, decorate application with non-weaving cloth (like wall paper, carpet) and energy-saving building materials fields such as (like plasterboard, concrete).
The technical scheme that the present invention adopts is: theoretical according to eutectic point; It at first is raw material with the LCFA; The method of utilizing melting mixing and sonic oscillation to combine prepares binary aliphatic acid eutectic, and adopting the method preparation of electrostatic spinning then is the latent heat of phase change and the regulatable fixed phase change superfine composite fiber of phase transition temperature of backing material with the polymer superfine fibre.
The preparation method of a kind of binary aliphatic acid/polymer fixed phase change superfine composite fiber comprises the steps:
(1) at first, select two kinds of LCFAs to mix, the aliphatic acid binary mixture that configures is placed in 50～100 ℃ the baking oven and is incubated 0.5～4h at the eutectic mass ratio.And then putting it into ultrasonic vibration 1～60min in the water-bath of ultrasonic generator, the temperature of control water-bath is about 50～90 ℃.At last, it is lowered the temperature naturally and obtain binary aliphatic acid eutectic.
(2) with polymer dissolution in single solvent or mixed solvent, be made into the polymer quality mark and be 5～20% spinning solution.Again the binary aliphatic acid eutectic that makes is dissolved in the spinning solution according to the certain quality ratio as the solid-liquid phase change material, fully stirs with magnetic stirring apparatus and form uniform composite spinning solution; The quality ratio range of described binary aliphatic acid eutectic and polymer is 5/100～250/100.
(3) in electrostatic spinning apparatus, spin uniform fixed phase change superfine composite fiber at last.The concrete technological parameter of described electrostatic spinning is: spinning voltage 5～60kV; Distance between spinning head and the receiving system is 5～40cm; The flow rate of liquid of spinning solution is 0.1～8ml/h, and receiving system is dull and stereotyped the reception or the cylinder reception, and drum rotation speed is 5～1000rpm; Ambient temperature is 5～40 ℃, and relative air humidity is 40～90%.The diameter Distribution scope of described fixed phase change superfine composite fiber is 50nm～10 μ m, and the phase transition temperature distribution is 14～80 ℃, and phase transformation enthalpy distribution is 5～250kJ/kg.
LCFA described in the step (1) is capric acid, laurate, myristic acid, palmitic acid, stearic acid etc.Described aliphatic acid eutectic is capric acid-laurate binary eutectic, capric acid-myristic acid binary eutectic, capric acid-palmitic acid binary eutectic, capric acid-stearic acid binary eutectic, laurate-myristic acid binary eutectic, laurate-palmitic acid binary eutectic, laurate-stearic acid binary eutectic, myristic acid-palmitic acid binary eutectic, myristic acid-stearic acid binary eutectic, palmitic acid-stearic acid binary eutectic etc.
Polymer support material described in the step (2) is PET, polymethyl methacrylate, polyamide, polyacrylonitrile, polyethylene glycol oxide, polyhexamethylene adipamide, polyurethane, PLA, cellulose acetate etc.Described solvent is N, one or both mixed solvents in dinethylformamide, DMAC N,N, acetone, oxolane, carrene, chloroform, trifluoroacetic acid, formic acid, the hexafluoroisopropanol.
Above-mentioned fixed phase change superfine composite fiber is expected to be widely used in indoor and decorates with non-weaving cloth (like wall paper, carpet) energy saving building material (like plasterboard, concrete), biology or various fields such as medical material, phase-change accumulation energy air-conditioning system, heat-accumulation temperature-adjustment fiber and function textile.
Because adopt technique scheme, the present invention has following advantage and effect:
1, binary aliphatic acid of the present invention/polymer fixed phase change energy-storage ultra-fine composite fiber; Both had lower phase transition temperature and higher latent heat of phase change; Simultaneously can be different according to the ratio of LCFA kind of selecting and aliphatic acid mixing; Phase transition temperature and latent heat of phase change to the aliphatic acid binary mixture carry out suitable regulation and control, make the phase transition temperature and the latent heat of phase change of the fixed phase change energy-storage ultra-fine composite fiber that makes different, enlarge its suitable application area in reality.
2, fixed phase change energy-storage ultra-fine composite fiber of the present invention is to be backing material with the polymer superfine fibre; Can solve the leakage problems of binary aliphatic acid eutectic effectively at phase transition process; Need not equipment packages, can directly use, thereby improved heat conductivity, reduced cost.
3, the electrospinning process of the present invention's employing is a kind of important technology of preparation micron order or nano level superfine polymer fiber, and it is simple to have technical process, and technological parameter is easy to advantages such as adjusting.The phase-change energy-storage ultra-fine composite fiber that adopts the method to make not only has good energy-saving and temperature-regulating effect, also has big, unique network configuration of specific area and abundant excellent properties such as porosity.
4, the LCFA wide material sources that adopt of the present invention and be prone to obtain have nontoxic non-corrosiveness, were not prone to that cold-peace is separated, latent heat of phase change big and advantage such as low price.The type of polymer that adopts is many, the source is wide, and all has better spinnability.The preparation method of binary aliphatic acid eutectic is simple simultaneously, safety is easy realizes.
Description of drawings
Fig. 1 is the SEM figure of the phase-change energy-storage ultra-fine composite fiber of instance 1 preparation.
Fig. 2 is thermal energy storage (DSC) curve of the phase-change energy-storage ultra-fine composite fiber of instance 1 preparation.
The specific embodiment
Below in conjunction with specific embodiment the present invention is explained further details, but the invention is not restricted to following embodiment.
At first, take by weighing laurate (LA) respectively and palmitic acid (PA) mixes according to 77.51: 22.49 eutectic quality proportioning, the mixture that configures is placed in 60 ℃ the baking oven and is incubated 1h with electronic balance.And then putting it into ultrasonic vibration 2min in the water-bath of ultrasonic generator, the temperature of control water-bath is about 60 ℃.At last, it is lowered the temperature naturally and obtain the LA-PA binary eutectic.
It is in carrene/trifluoroacetic acid mixed solvent of 2: 1 that PET (PET) is dissolved in volume ratio, is made into the PET mass fraction and is 15% solution.Then the LA-PA eutectic for preparing is dissolved in the PET solution, is mixed with the LA-PA/PET mass ratio and is 50/100 composite spinning liquid, it is mixed with magnetic stirrer.The composite spinning liquid for preparing is carried out spinning through electrostatic spinning apparatus, is receiving system with the cylinder, and spinning head is 18cm to the receiving range of cylinder, spinning solution to feed to speed be 2ml/h, spinning voltage is 16kV.Environment temperature is 20 ℃ in the spinning process, and relative humidity is 60%.At ambient temperature, the fibrofelt for preparing is placed in the vacuum drying chamber dry 24h to remove residual solvent.
Average diameter through SEM test phase-change accumulation energy composite ultrafine fiber is 992nm; Through its fusion temperature of DSC measuring technology analysis is 36.62 ℃, and crystallization temperature is 30.75 ℃, and fusion enthalpy is 33.94kJ/kg, and the crystallization enthalpy is 36.21kJ/kg.
At first, take by weighing palmitic acid (PA) respectively and myristic acid (MA) mixes according to 66.92: 33.08 eutectic quality proportioning, the mixture that configures is placed in 70 ℃ the baking oven and is incubated 2h with electronic balance.And then putting it into ultrasonic vibration 5min in the water-bath of ultrasonic generator, the temperature of control water-bath is about 70 ℃.At last, it is lowered the temperature naturally and obtain the PA-MA binary eutectic.
It is in carrene/trifluoroacetic acid mixed solvent of 2: 1 that PET (PET) is dissolved in volume ratio, is made into the PET mass fraction and is 15% solution.Then the PA-MA eutectic for preparing is dissolved in the PET solution, is mixed with the PA-MA/PET mass ratio and is 100/100 composite spinning liquid, it is mixed with magnetic stirrer.The composite spinning liquid for preparing is carried out spinning through electrostatic spinning apparatus, is receiving system with the cylinder, and spinning head is 20cm to the receiving range of cylinder, spinning solution to feed to speed be 3ml/h, spinning voltage is 18kV.Environment temperature is 25 ℃ in the spinning process, and relative humidity is 70%.At ambient temperature, the fibrofelt for preparing is placed in the vacuum drying chamber dry 24h to remove residual solvent.
Average diameter through SEM test phase-change accumulation energy composite ultrafine fiber is 2178nm; Through its fusion temperature of DSC measuring technology analysis is 46.83 ℃, and crystallization temperature is 42.17 ℃, and fusion enthalpy is 87.89kJ/kg, and the crystallization enthalpy is 79.64kJ/kg.
Embodiment 3
At first, take by weighing palmitic acid (PA) respectively and stearic acid (SA) mixes according to 62.99: 37.01 eutectic quality proportioning, the mixture that configures is placed in 90 ℃ the baking oven and is incubated 2h with electronic balance.And then putting it into ultrasonic vibration 2min in the water-bath of ultrasonic generator, the temperature of control ultrasound bath is about 90 ℃.At last, it is cooled off naturally and obtain the PA-SA binary eutectic.
It is in carrene/trifluoroacetic acid mixed solvent of 1: 1 that PET (PET) is dissolved in volume ratio, is made into the PET mass fraction and is 10% solution.Then the PA-SA eutectic for preparing is dissolved in the PET solution, is mixed with the PA-SA/PET mass ratio and is 150/100 composite spinning liquid, it is mixed with magnetic stirrer.The composite spinning liquid for preparing is carried out spinning through electrostatic spinning apparatus, is receiving system with the cylinder, and spinning head is 15cm to the receiving range of cylinder, spinning solution to feed to speed be 5ml/h, spinning voltage is 20kV.Environment temperature is 30 ℃ in the spinning process, and relative humidity is 80%.At ambient temperature, the fibrofelt for preparing is placed in the vacuum drying chamber dry 24h to remove residual solvent.
Average diameter through SEM test phase-change accumulation energy composite ultrafine fiber is 4917nm; Through its fusion temperature of DSC measuring technology analysis is 56.21 ℃, and crystallization temperature is 51.68 ℃, and fusion enthalpy is 130.7kJ/kg, and the crystallization enthalpy is 110.5kJ/kg.
Claims (6)
1. aliphatic acid/polymer fixed phase change superfine composite fiber; It is characterized in that with the LCFA being raw material; The mode that adopts melting mixing and sonic oscillation to combine prepares binary aliphatic acid as the solid-liquid phase change material; Utilize the technology and the principle of electrostatic spinning; Preparation is backing material, the regulatable fixed phase change superfine composite fiber of phase transition temperature with the polymer superfine fibre, and described binary fatty acid profile is on the surface of polymer superfine fibre and inner, is that the effect through hydrogen bond combines between phase change material and the polymer.
2. a kind of aliphatic acid according to claim 1/polymer fixed phase change superfine composite fiber is characterized in that: the latent heat of phase change of described fixed phase change superfine composite fiber and phase transition temperature are can be according to the ratio that the LCFA kind of selecting and aliphatic acid mix different to be regulated and control.
3. a kind of aliphatic acid according to claim 1/polymer fixed phase change superfine composite fiber; It is characterized in that: the diameter Distribution scope of described fixed phase change superfine composite fiber is 50nm～10 μ m; The phase transition temperature distribution is 14～80 ℃, and the latent heat of phase change distribution is 5～250kJ/kg.
4. the preparation method of aliphatic acid/polymer fixed phase change superfine composite fiber comprises the steps:
(1) at first, select two kinds of LCFAs to mix, the aliphatic acid binary mixture for preparing is placed in 50～100 ℃ the baking oven and is incubated 0.5～4h at the eutectic mass ratio.And then putting it into ultrasonic vibration 1～60min in the water-bath of ultrasonic generator, the temperature of control water-bath is about 50～90 ℃.At last, it is lowered the temperature naturally and obtain binary aliphatic acid eutectic;
(2) with polymer dissolution in solvent, be made into the polymer quality mark and be 5～20% spinning solution.Again the binary aliphatic acid eutectic that makes is dissolved in the spinning solution according to the certain quality ratio as the solid-liquid phase change material, fully stirs with magnetic stirring apparatus and form uniform composite spinning solution; The quality ratio range of described binary aliphatic acid eutectic and polymer is 5/100～250/100;
(3) will mix spinning solution and carry out spinning, obtain the fixed phase change superfine composite fiber of diameter between 50nm～10 μ m through the high-voltage electrostatic spinning method.The concrete technological parameter of described electrostatic spinning is: spinning voltage 5～60kV; Distance between spinning head and the receiving system is 5～40cm; The flow rate of liquid of spinning solution is 0.1～8ml/h, and receiving system is flat board or cylinder, and drum rotation speed is 5～1000rpm; Ambient temperature is 5～40 ℃, and relative air humidity is 40～90%.
5. the preparation method of a kind of binary aliphatic acid according to claim 4/polymer fixed phase change superfine composite fiber is characterized in that: the described LCFA of step (1) is capric acid, laurate, myristic acid, palmitic acid, stearic acid etc.Described binary aliphatic acid is capric acid-laurate binary eutectic, capric acid-myristic acid binary eutectic, capric acid-palmitic acid binary eutectic, capric acid-stearic acid binary eutectic, laurate-myristic acid binary eutectic, laurate-palmitic acid binary eutectic, laurate-stearic acid binary eutectic, myristic acid-palmitic acid binary eutectic, myristic acid-stearic acid binary eutectic, palmitic acid-stearic acid binary eutectic etc.;
Polymer support material described in the step (2) is PET, polymethyl methacrylate, polyamide, polyacrylonitrile, polyethylene glycol oxide, polyhexamethylene adipamide, polyurethane, PLA, cellulose acetate etc.Described solvent is N, one or both mixed solvents in dinethylformamide, DMAC N,N, acetone, oxolane, carrene, chloroform, trifluoroacetic acid, formic acid, the hexafluoroisopropanol.
6. can be widely used in indoor according to the said binary aliphatic acid of claim 1/polymer fixed phase change superfine composite fiber and decorate with non-weaving cloth (like wall paper, carpet), energy-saving building materials (like plasterboard, concrete), biology or various fields such as medical material, phase-change accumulation energy air-conditioning system, heat-accumulation temperature-adjustment fiber and function textile.
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| CN114855361A (en) * | 2022-05-20 | 2022-08-05 | 中原工学院 | Fluorine-free environment-friendly waterproof moisture-permeable nanofiber membrane based on thermal regulation and preparation method thereof |
| CN116590806A (en) * | 2023-04-12 | 2023-08-15 | 华南理工大学 | Binary fatty acid eutectic composite fiber capable of magnetic resonance imaging and preparation and application thereof |
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Application publication date: 20120725 |