CN100447315C - Super fine composite terylene fibers storing energy through phase change, and preparation method - Google Patents
Super fine composite terylene fibers storing energy through phase change, and preparation method Download PDFInfo
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- CN100447315C CN100447315C CNB200610037169XA CN200610037169A CN100447315C CN 100447315 C CN100447315 C CN 100447315C CN B200610037169X A CNB200610037169X A CN B200610037169XA CN 200610037169 A CN200610037169 A CN 200610037169A CN 100447315 C CN100447315 C CN 100447315C
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Abstract
The present invention discloses a phase-transition energy storage superfine composite, polyester fibre and its preparation method. Said phase-transition energy storage superfine composite polyester fibre is made up by using polyester fibre as carrier and using stearic acid and its ester derivative as phase-transition material through a high-voltage static field spinning preparation process. The described phase-transition material is covered in the interior of said polyester fibre base body, in which the described polyester fibre content is 50-95% of total mass, and the described phase-transition material content is 5-50% of total mass. It can be used as functional material and can be extensively used in the field of various materials.
Description
Technical field
The present invention relates to the phase-change material field, particularly a kind of super fine composite terylene fibers storing energy through phase change and preparation method thereof.
Background technology
Phase-change material is a kind of energy storage material of extensive use, and along with the arrival of energy crisis, the application of phase-change material is with even more important.According to the difference of phase transformation mode, the phase-change material of practical application mainly is divided into solid-liquid phase change material and solid-solid phase transition material.
Phase change fiber is a kind of solid-solid phase transition material, and is a kind of novel intelligent function material.At present, phase change fiber mainly comprises following several form: (1) phase-change material is filled or is injected in the doughnut, and U.S. scientist Vigo and Frost just adopt the synthetic fiber with the aqueous solution injection hollow of hydrated inorganic salt, polyethylene glycol and polyalcohol to make this phase change fiber material; (2) phase-change material covered fiber, people such as U.S. scientist Vigo have studied the crosslinked covered fiber of phase-change material polyethylene glycol and have obtained practical application, people such as Zuckerman and Umible adopt phase-change material micro-capsule by binding agent fixedly the method for covered fiber made phase change fiber; (3) sneak into phase-change material in the fibre spinning process, people such as the Zhang Xingxiang of Tianjin University of Technology adopt this method to prepare the fibrous material that the mixture of polyethylene glycol and ethylene-vinyl acetate copolymer and the block copolymer of polyethylene glycol and polyethylene terephthalate etc. have the phase transformation performance, Bryant and Colvin etc. make phase change fiber to phase-change material micro-capsule and the spinning of spinning material mixed melting, but this fiber is a conventional fibre, and general diameter is more than micron and less stable.
Method of electrostatic spinning is a kind of method for preparing superfine fibre of novelty, and the fibre diameter that makes with this method generally arrives hundreds of nanometers tens.People such as the Chen Yan of Donghua University mould have reported a kind of preparation and application of phase transformation composite electrostatic spinning stoste in publication number is the patent of CN 1493720A.But the research that utilizes the method for electrostatic spinning preparation to have the dacron ultrafine fiber of phase-change thermal storage function does not appear in the newspapers as yet.
Summary of the invention
The objective of the invention is to overcome the shortcoming that exists in the prior art, a kind of Heat stability is good is provided, the super fine composite terylene fibers storing energy through phase change that micromolecule leaks, outward appearance is stable, solid does not take place.
Another object of the present invention is to provide a kind of preparation method of above-mentioned super fine composite terylene fibers storing energy through phase change.
Purpose of the present invention is achieved through the following technical solutions:
A kind of super fine composite terylene fibers storing energy through phase change is a carrier with the terylene, is phase-change material with stearic acid and ester derivative thereof, and described phase-change material is covered by terylene base material inside; Wherein said terylene accounts for 50～95% of gross mass, and described phase-change material accounts for 5～50% of gross mass.
Described stearic acid and ester derivative thereof are hydrophobic, preferred stearic acid, butanediol distearate, glycol distearate, hexylene glycol distearate, pentaerythritol tetrastearate, alkyl amino distearate or the amino distearate of aromatic radical etc.
The average fibre diameter of described super fine composite terylene fibers storing energy through phase change is 500～900nm, and fibre morphology is the nonwoven fabric form.
The preparation method of above-mentioned super fine composite terylene fibers storing energy through phase change comprises the steps: at first terylene to be dissolved in the solvent, adds phase-change material then, stirs to obtain even mixed solution; Again described mixed solution is carried out the high-voltage electrostatic field spinning, obtain super fine composite terylene fibers storing energy through phase change.
Described solvent is a trifluoroacetic acid.
The spinning of described high-voltage electrostatic field is described mixed solution to be packed into have in the syringe of spinning head, make described mixed solution constant speed arrive spinning head by the sampling pump pushing syringe, carry out electrostatic spinning then, and collect the superfine fibre spun with collecting board, remove residual solvent with boulton process again, obtain super fine composite terylene fibers storing energy through phase change.
In the spinning of described high-voltage electrostatic field, spinning voltage is 15～40KV, and the distance between spinning head and the collecting board is 10～30cm, and the sample introduction flow velocity of described mixed solution is 0.1～20mL/h, and ambient temperature is 20～25 ℃, and relative humidity is 45～85%.
The phase transition temperature of the super fine composite terylene fibers storing energy through phase change of the present invention's preparation is 0～80 ℃, and enthalpy of phase change is 10～100kJ/kg; And all can keep solid shape before and after the phase transformation, any micromolecular leakage can not take place.The quality proportioning of kind, phase-change material and terylene that can be by changing phase-change material is regulated the enthalpy of phase change of super fine composite terylene fibers storing energy through phase change.Because the phase-change material that the present invention adopts is the lyophobic dust that contains chain alkyl and ester group, carrier is chemically inert terylene base material, so phase-change material and carrier have certain compatibility.
The present invention compared with prior art has following advantage and effect:
(1) Heat stability is good of super fine composite terylene fibers storing energy through phase change of the present invention, micromolecule phase-change material are covered by terylene base material inside, do not leak, and outward appearance are stable, solid.
(2) super fine composite terylene fibers storing energy through phase change surface texture of the present invention is regular, micromolecule phase-change material and terylene base material intermiscibility are good, phase-change material and terylene base material mass ratio are 1: reach the purpose of adjusting the phase-change accumulation energy size, enthalpy of phase change height thereby can regulate arbitrarily below 1.
(3) super fine composite terylene fibers storing energy through phase change of the present invention has the characteristic of superfine fibre and phase-change accumulation energy simultaneously, can be used as functional material and is applied to each field.
(4) average diameter of super fine composite terylene fibers storing energy through phase change of the present invention is 500nm～900nm, has bigger specific area, high porosity, good permeability, excellent mechanical property and adjustment performance.
(5) preparation technology of the present invention is simple, and is workable.
Description of drawings
Fig. 1 is the Electronic Speculum figure of the super fine composite terylene fibers storing energy through phase change of embodiment 1 preparation.
Fig. 2 is the Electronic Speculum figure of the super fine composite terylene fibers storing energy through phase change of embodiment 2 preparations.
The specific embodiment
Below in conjunction with embodiment the present invention is done further detailed description, but embodiments of the present invention are not limited thereto.
Embodiment 1:
At first terylene short fiber peacekeeping trifluoroacetic acid is pressed mass ratio and mixed at 1: 5, add the phase-change material stearic acid then, and make phase-change material account for 25% of phase-change material and terylene gross mass, obtain even mixed solution after the mechanical agitation; Externally environment temperature is that 25 ℃, relative humidity are 85%, the electrostatic field spinning voltage is that distance between 15KV, spinning head and the collecting board is to carry out the high-voltage electrostatic field spinning under the condition of 10cm with mixed solution again, being about to mixed solution packs into and has in the syringe of spinning head, make mixed solution arrive spinning head by the sampling pump pushing syringe with the sample introduction flow velocity constant speed of 1mL/h, carry out electrostatic spinning then, and collect the superfine fibre spun with collecting board, remove residual trifluoroacetic acid with vacuumize again, obtain super fine composite terylene fibers storing energy through phase change at last.
Differential thermal analysis (DSC) result shows the phase transformation onset temperature of this kind super fine composite terylene fibers storing energy through phase change at 56.9 ℃, and enthalpy of phase change is 46.5kJ/kg.
Embodiment 2:
At first terylene short fiber peacekeeping trifluoroacetic acid is pressed mass ratio and mixed at 1: 5, add phase-change material butanediol distearate then, and make phase-change material account for 10% of phase-change material and terylene gross mass, obtain even mixed solution after the mechanical agitation; Externally environment temperature is that 22 ℃, relative humidity are 65%, the electrostatic field spinning voltage is that distance between 20KV, spinning head and the collecting board is to carry out the high-voltage electrostatic field spinning under the condition of 15cm with mixed solution again, being about to mixed solution packs into and has in the syringe of spinning head, make mixed solution arrive spinning head by the sampling pump pushing syringe with the sample introduction flow velocity constant speed of 0.2mL/h, carry out electrostatic spinning then, and collect the superfine fibre spun with collecting board, remove residual trifluoroacetic acid with vacuumize again, obtain super fine composite terylene fibers storing energy through phase change at last.
Differential thermal analysis (DSC) result shows the phase transformation onset temperature of this kind super fine composite terylene fibers storing energy through phase change at 41.2 ℃, and enthalpy of phase change is 14.2kJ/kg.
Embodiment 3:
At first terylene short fiber peacekeeping trifluoroacetic acid is pressed mass ratio and mixed at 1: 5, add phase-change material hexylene glycol distearate then, and make phase-change material account for 48% of phase-change material and terylene gross mass, obtain even mixed solution after the mechanical agitation; Externally environment temperature is that 21 ℃, relative humidity are 45%, the electrostatic field spinning voltage is that distance between 22KV, spinning head and the collecting board is to carry out the high-voltage electrostatic field spinning under the condition of 13cm with mixed solution again, being about to mixed solution packs into and has in the syringe of spinning head, make mixed solution arrive spinning head by the sampling pump pushing syringe with the sample introduction flow velocity constant speed of 15mL/h, carry out electrostatic spinning then, and collect the superfine fibre spun with collecting board, remove residual trifluoroacetic acid with vacuumize again, obtain super fine composite terylene fibers storing energy through phase change at last.
Differential thermal analysis (DSC) result shows the phase transformation onset temperature of this kind super fine composite terylene fibers storing energy through phase change at 38.8 ℃, and enthalpy of phase change is 80.3kJ/kg.
Embodiment 4:
At first terylene short fiber peacekeeping trifluoroacetic acid is pressed mass ratio and mixed at 1: 5, add the phase-change material pentaerythritol tetrastearate then, and make phase-change material account for 15% of phase-change material and terylene gross mass, obtain even mixed solution after the mechanical agitation; Externally environment temperature is that 22 ℃, relative humidity are 65%, the electrostatic field spinning voltage is that distance between 20KV, spinning head and the collecting board is to carry out the high-voltage electrostatic field spinning under the condition of 11cm with mixed solution again, being about to mixed solution packs into and has in the syringe of spinning head, make mixed solution arrive spinning head by the sampling pump pushing syringe with the sample introduction flow velocity constant speed of 0.5mL/h, carry out electrostatic spinning then, and collect the superfine fibre spun with collecting board, remove residual trifluoroacetic acid with vacuumize again, obtain super fine composite terylene fibers storing energy through phase change at last.
Differential thermal analysis (DSC) result shows the phase transformation onset temperature of this kind super fine composite terylene fibers storing energy through phase change at 39.5 ℃, and enthalpy of phase change is 24.5kJ/kg.
Embodiment 5:
At first terylene short fiber peacekeeping trifluoroacetic acid is pressed mass ratio and mixed at 1: 5, add phase-change material hexa-methylene diamino stearate then, and make phase-change material account for 20% of phase-change material and terylene gross mass, obtain even mixed solution after the mechanical agitation; Externally environment temperature is that 24 ℃, relative humidity are 55%, the electrostatic field spinning voltage is that distance between 18KV, spinning head and the collecting board is to carry out the high-voltage electrostatic field spinning under the condition of 15cm with mixed solution again, being about to mixed solution packs into and has in the syringe of spinning head, make mixed solution arrive spinning head by the sampling pump pushing syringe with the sample introduction flow velocity constant speed of 11mL/h, carry out electrostatic spinning then, and collect the superfine fibre spun with collecting board, remove residual trifluoroacetic acid with vacuumize again, obtain super fine composite terylene fibers storing energy through phase change at last.
Differential thermal analysis (DSC) result shows the phase transformation onset temperature of this kind super fine composite terylene fibers storing energy through phase change at 58.2 ℃, and enthalpy of phase change is 24.5kJ/kg.
Embodiment 6:
At first terylene short fiber peacekeeping trifluoroacetic acid is pressed mass ratio and mixed at 1: 5, add the phase-change material glycol distearate then, and make phase-change material account for 45% of phase-change material and terylene gross mass, obtain even mixed solution after the mechanical agitation; Externally environment temperature is that 20 ℃, relative humidity are 50%, the electrostatic field spinning voltage is that distance between 25KV, spinning head and the collecting board is to carry out the high-voltage electrostatic field spinning under the condition of 14cm with mixed solution again, being about to mixed solution packs into and has in the syringe of spinning head, make mixed solution arrive spinning head by the sampling pump pushing syringe with the sample introduction flow velocity constant speed of 20mL/h, carry out electrostatic spinning then, and collect the superfine fibre spun with collecting board, remove residual trifluoroacetic acid with vacuumize again, obtain super fine composite terylene fibers storing energy through phase change at last.
Differential thermal analysis (DSC) result shows the phase transformation onset temperature of this kind super fine composite terylene fibers storing energy through phase change at 37.8 ℃, and enthalpy of phase change is 88.1kJ/kg.
Embodiment 7:
At first terylene short fiber peacekeeping trifluoroacetic acid is pressed mass ratio mixes at 1: 5, add phase-change material 4 then, 4 '-diphenyl methane diaminourea stearate, and make phase-change material account for 31% of phase-change material and terylene gross mass, obtain even mixed solution after the mechanical agitation; Externally environment temperature is that 25 ℃, relative humidity are 60%, the electrostatic field spinning voltage is that distance between 20KV, spinning head and the collecting board is to carry out the high-voltage electrostatic field spinning under the condition of 15cm with mixed solution again, being about to mixed solution packs into and has in the syringe of spinning head, make mixed solution arrive spinning head by the sampling pump pushing syringe with the sample introduction flow velocity constant speed of 0.9mL/h, carry out electrostatic spinning then, and collect the superfine fibre spun with collecting board, remove residual trifluoroacetic acid with vacuumize again, obtain super fine composite terylene fibers storing energy through phase change at last.
Differential thermal analysis (DSC) result shows the phase transformation onset temperature of this kind super fine composite terylene fibers storing energy through phase change at 61.7 ℃, and enthalpy of phase change is 31.0kJ/kg.
Claims (6)
1, a kind of super fine composite terylene fibers storing energy through phase change is characterized in that: being carrier with the terylene, is phase-change material with stearic acid or its ester derivative, and described phase-change material is covered by terylene base material inside; Wherein said terylene accounts for 50～95% of gross mass; Described phase-change material accounts for 5～50% of gross mass; The average fibre diameter of described super fine composite terylene fibers storing energy through phase change is 500～900nm.
2, super fine composite terylene fibers storing energy through phase change according to claim 1 is characterized in that: described stearic acid or its ester derivative are stearic acid, butanediol distearate, glycol distearate, hexylene glycol distearate or pentaerythritol tetrastearate.
3, a kind of preparation method of each described super fine composite terylene fibers storing energy through phase change of claim 1～2 is characterized in that comprising the steps: at first terylene being dissolved in the solvent, adds phase-change material then, stirs to obtain even mixed solution; Again described mixed solution is carried out the high-voltage electrostatic field spinning, spinning voltage is 15～40KV, obtains super fine composite terylene fibers storing energy through phase change.
4, the preparation method of super fine composite terylene fibers storing energy through phase change according to claim 3 is characterized in that: described solvent is a trifluoroacetic acid.
5, the preparation method of super fine composite terylene fibers storing energy through phase change according to claim 3, it is characterized in that: the spinning of described high-voltage electrostatic field is described mixed solution to be packed into have in the syringe of spinning head, make described mixed solution constant speed arrive spinning head by the sampling pump pushing syringe, carry out electrostatic spinning then, and collect the superfine fibre spun with collecting board, remove residual solvent with vacuumize again, obtain super fine composite terylene fibers storing energy through phase change.
6, according to the preparation method of claim 3 or 5 described super fine composite terylene fibers storing energy through phase change, it is characterized in that: in the spinning of described high-voltage electrostatic field, distance between spinning head and the collecting board is 10～30cm, the sample introduction flow velocity of described mixed solution is 0.1～20mL/h, ambient temperature is 20～25 ℃, and relative humidity is 45～85%.
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| CN100593559C (en) * | 2007-06-22 | 2010-03-10 | 中国科学院化学研究所 | Phase-change material of natural kawo fiber pipe encapsulation and encapsulation method thereof |
| CN101684403B (en) * | 2008-09-25 | 2013-03-20 | 中国科学院化学研究所 | Phase change material microcapsules encapsulated by natural microtubules and preparation method thereof |
| CN103710964B (en) * | 2013-12-18 | 2015-12-02 | 中国皮革和制鞋工业研究院 | A kind of preparation method of phase change fiber |
| CN105019053B (en) * | 2015-07-03 | 2017-06-23 | 山西瑞赛格纺织科技有限公司 | One kind can weave phase-change accumulation energy polyster fibre |
| CN114644526B (en) * | 2022-04-22 | 2022-11-29 | 江苏瑞复达高温新材料股份有限公司 | Rapid baking structural ceramic for aluminum industrial furnace and preparation method thereof |
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| CN1908258A (en) * | 2006-08-10 | 2007-02-07 | 中国科学院广州化学研究所 | Phase-change energy-storage ultra-fine composite fiber and preparation method and application thereof |
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| US20020011587A1 (en) * | 2000-07-03 | 2002-01-31 | Suppes Galen J. | Fatty-acid thermal storage devices, cycle, and chemicals |
| CN1493720A (en) * | 2003-07-02 | 2004-05-05 | 东华大学 | Phase change composite spinning solution and its preparation and application |
| CN1710012A (en) * | 2005-06-29 | 2005-12-21 | 中国科学院广州化学研究所 | Nano cellulose solid-solid phase transition material and its preparing method |
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