CN107447294A - A kind of method that PEG/PET solid-solid phase change materials are prepared using electrostatic spinning technique - Google Patents

A kind of method that PEG/PET solid-solid phase change materials are prepared using electrostatic spinning technique Download PDF

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Publication number
CN107447294A
CN107447294A CN201710776738.0A CN201710776738A CN107447294A CN 107447294 A CN107447294 A CN 107447294A CN 201710776738 A CN201710776738 A CN 201710776738A CN 107447294 A CN107447294 A CN 107447294A
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CN
China
Prior art keywords
peg
pet
solid
solution
electrostatic spinning
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Pending
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CN201710776738.0A
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Chinese (zh)
Inventor
王瑶
崔学伟
唐建国
刘继宪
黄林军
焦吉庆
王彦欣
王薇
韩真真
邢丽
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Qingdao University
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Qingdao University
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Priority to CN201710776738.0A priority Critical patent/CN107447294A/en
Publication of CN107447294A publication Critical patent/CN107447294A/en
Pending legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/04—Melting filament-forming substances
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention discloses a kind of method that PEG/PET solid-solid phase change materials are prepared using electrostatic spinning technique, comprise the following steps：PET is dissolved in dichloromethane first：In trifluoroacetic acid mixed solution, 5~10 hours under magnetic stirring, after it is completely dissolved, according to mass ratio PET：PEG=4:1‑1:1 adds PEG, equally under magnetic stirring 5~10 hours, PEG is also dissolved in solution；The solution of gained is subjected to electrostatic spinning under 20~25 degrees Celsius, 16~20kV of voltage, 0.05~0.15mL/min of solution speed, receives under the conditions of distance is 18~20cm and carries out spinning.The invention is using PET as skeletal support material, polyethylene glycol is phase-change material, the heat content for the solid-solid phase change material that two kinds of materials are mixed to form reaches as high as 146.8J/g, this causes polyethylene glycol while high thermal energy storage is kept, also make transformation of its change procedure without phase, effectively prevent the leakage problem of phase-change material.

Description

A kind of method that PEG/PET solid-solid phase change materials are prepared using electrostatic spinning technique
Technical field
The present invention relates to technical field of phase-change energy storage, and it is solid to prepare PEG/PET in particular with electrostatic spinning technique The method of phase change materials.
Background technology
Phase-change material is that one kind can be undergone phase transition in small temperature range, so as to reach a large amount of energy stores and release Material.Every field of the phase-change material in life has to be widely applied very much, and prospect is considerable, for example, astronaut's clothes On phase-change material, solar energy storage, phase-change material substitutes compressor etc. on the house insulation of building field, refrigeration plant.So And traditional phase-change material shortcoming is clearly, solid-liquid phase change materials are easily revealed when storing heat energy, therefore, can be with The solid-solid phase change material of leakage is effectively prevented to be more exposed to everybody concern.
Polyethylene glycol is a kind of to possess the phase-change material that big heat content, fusing point are appropriate, wearability is good, simple polyethylene glycol Solid-liquid phase change material can only be used as, is easily revealed, using limited.PET is a kind of thermoplasticity, wearability, corrosion resistance, resistance to Hot, intensity is all very good, and applies quite varied material.The present invention is using the method for electrostatic spinning by PET and difference The PEG of molecular weight carries out being mixed with solid-solid phase change material, while the material possesses high enthalpy, can prevent well it is solid- Leakage during liquid phase change.
The content of the invention
It is an object of the invention to provide a kind of side that PEG/PET solid-solid phase change materials are prepared using electrostatic spinning technique Method.
The present invention is achieved through the following technical solutions：
A kind of method that PEG/PET solid-solid phase change materials are prepared using electrostatic spinning technique, is comprised the following steps：
The preparation of PEG/PET electrostatic spinning solutions：PET is dissolved in dichloromethane first：In trifluoroacetic acid mixed solution, 5~10 hours under magnetic stirring, after it is completely dissolved, according to mass ratio PET：PEG=4:1-1:1 adds PEG, equally exists 5~10 hours under magnetic agitation, PEG is set also to be dissolved in solution；
Electrostatic spinning prepares solid-solid phase change material：The solution of gained is subjected to electrostatic spinning under 20~25 degrees Celsius, electricity 16~20kV, 0.05~0.15mL/min of solution speed are pressed, receives under the conditions of distance is 18~20cm and carries out spinning.
Described method, dichloromethane：Both volume ratios are 2 in trifluoroacetic acid mixed solution:1.
Described method, the PEG used (polyethylene glycol) molecular weight are PEG6000 or PEG8000 or PEG10000.
Described method, the mass fractions of PET in the solution are 10wt% or 15wt% or 20wt% or 25wt%.
Described method, magnetic stirrer bar rotating speed are 500-800r/min.
Compared with original polyethylene glycol phase change materials, the present invention has advantages below：
1st, the present invention is successfully mixed PEG and PET so that as phase-change material by the method for electrostatic spinning PEG remain in that high heat content up to 146.8J/g, at the same time, can be good at preventing letting out in phase transition process PEG Dew.
2nd, the present invention use good biocompatibility PET and PEG, and whole process small toxicity, pollution is low, cost is low, Effect is good.
Brief description of the drawings
Fig. 1 is the scanning figure of electrospun fibers prepared by the inventive method；
Fig. 2 is the infrared curve for the electrospun fibers that the inventive method is prepared；
Fig. 3 is the DSC curve for the electrospun fibers that the inventive method is prepared；
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
The invention discloses a kind of method that PEG/PET solid-solid phase change materials are prepared using electrostatic spinning technique, its side Method step is as follows：
The preparation of PEG/PET electrostatic spinning solutions：The PET that 4.0g viscosity is 0.675dL/g is dissolved in volume ratio first For 2:1 dichloromethane：In trifluoroacetic acid solution, 10 hours under magnetic stirring, after it is completely dissolved, 1.0g molecules are added The PEG of amount 8000, equally under magnetic stirring 10 hours, makes PEG also be dissolved in solution.Then the solution of gained is taken the photograph 25 Electrostatic spinning is carried out under family name's degree.
Electrostatic spinning prepares solid-solid phase change material：By the PEG/PET electrostatic spinning solutions of gained, in voltage 19kV, solution Speed 0.15mL/min, receive under the conditions of distance is 18cm and carry out spinning.
The mass fractions of PET in the solution are 10wt% in the present embodiment.
Wherein, magnetic stirrer bar rotating speed is 600r/min.
By the scanning map analysis to phase-change material, see Fig. 1, about 1.5 microns~2 microns of electrospun fibers diameter it Between, and surface is smooth, without obvious adhesion or rat, illustrates that PET and PEG compatibilities are fine, can lead to well Electrostatic spinning is crossed to mix.
By infrared analysis, Fig. 2 is seen, PET some characteristic peaks and PEG characteristic peak all appear in infrared figure well In spectrum, it was demonstrated that PET and PEG is in the fiber of electrostatic spinning.
By differential scanning calorimetery (DSC), Fig. 3 is seen, it can be seen that the phase of the phase change materials prepared by the present embodiment In transition process, heat content is up to 146.8J/g, and the process is solid solid transformation without revealing.
Embodiment 2
The preparation of PEG/PET electrostatic spinning solutions：The PET that 4.0g viscosity is 0.675dL/g is dissolved in volume ratio first For 2:1 dichloromethane：In trifluoroacetic acid solution, 10 hours under magnetic stirring, after it is completely dissolved, 4.0g molecules are added The PEG of amount 6000, equally under magnetic stirring 10 hours, makes PEG also be dissolved in solution.Then the solution of gained is taken the photograph 20 Electrostatic spinning is carried out under family name's degree.
Electrostatic spinning prepares solid-solid phase change material：By the PEG/PET electrostatic spinning solutions of gained, in voltage 16kV, solution Speed 0.05mL/min, receive under the conditions of distance is 20cm and carry out spinning.
The mass fractions of PET in the solution are 15wt% in the present embodiment.
Wherein, magnetic stirrer bar rotating speed is 800r/min.
During the phase in version of phase change materials prepared by the present embodiment, heat content is up to 126.1J/g.
Embodiment 3
The preparation of PEG/PET electrostatic spinning solutions：The PET that 4.0g viscosity is 0.675dL/g is dissolved in volume ratio first For 2:1 dichloromethane：In trifluoroacetic acid solution, 10 hours under magnetic stirring, after it is completely dissolved, 1.0g molecules are added The PEG of amount 10000, equally under magnetic stirring 10 hours, makes PEG also be dissolved in solution.Then by the solution of gained 20 Electrostatic spinning is carried out under degree Celsius.
Electrostatic spinning prepares solid-solid phase change material：By the PEG/PET electrostatic spinning solutions of gained, in voltage 20kV, solution Speed 0.10mL/min, receive under the conditions of distance is 20cm and carry out spinning.
In the present embodiment, the mass fractions of PET in the solution are 20wt%.
Wherein, magnetic stirrer bar rotating speed is 500r/min.
During the phase in version of phase change materials prepared by the present embodiment, heat content is up to 131.4J/g.
It should be appreciated that for those of ordinary skills, can according to the above description be improved or converted, And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.

Claims (5)

  1. A kind of 1. method that PEG/PET solid-solid phase change materials are prepared using electrostatic spinning technique, it is characterised in that including following Step：
    The preparation of PEG/PET electrostatic spinning solutions：PET is dissolved in dichloromethane first：In trifluoroacetic acid mixed solution, in magnetic Power stirring is lower 5~10 hours, after it is completely dissolved, according to mass ratio PET：PEG=4:1-1:1 adds PEG, equally in magnetic force Stirring is lower 5~10 hours, PEG is also dissolved in solution；
    Electrostatic spinning prepares solid-solid phase change material：The solution of gained is subjected to electrostatic spinning, voltage 16 under 20~25 degrees Celsius ~20kV, 0.05~0.15mL/min of solution speed, receive under the conditions of distance is 18~20cm and carry out spinning.
  2. 2. the method as described in claim 1, it is characterised in that：Dichloromethane：Both volume ratios in trifluoroacetic acid mixed solution For 2:1.
  3. 3. the method as described in claim 1, it is characterised in that：PEG (polyethylene glycol) molecular weight used be PEG6000 or PEG8000 or PEG10000.
  4. 4. the method as described in claim 1, it is characterised in that：The mass fractions of PET in the solution are 10wt% or 15wt% Or 20wt% or 25wt%.
  5. 5. the method as described in claim 1, it is characterised in that：Magnetic stirrer bar rotating speed is 500-800r/min.
CN201710776738.0A 2017-09-01 2017-09-01 A kind of method that PEG/PET solid-solid phase change materials are prepared using electrostatic spinning technique Pending CN107447294A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108642599A (en) * 2018-04-24 2018-10-12 苏州龙杰特种纤维股份有限公司 A kind of phase change fiber and preparation method thereof
CN113393958A (en) * 2021-06-17 2021-09-14 山东大学 Transparent flexible electrode with ordered grid structure and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN101376702A (en) * 2008-10-09 2009-03-04 东华大学 Polyester based phase-change material having uvioresistant function and preparation thereof
CN104562292A (en) * 2014-12-29 2015-04-29 河南工程学院 Preparation method of porous micro-nano PET fibers
CN105019053A (en) * 2015-07-03 2015-11-04 山西瑞赛格纺织科技有限公司 Weaving phase-change energy-storage polyester fiber

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN101376702A (en) * 2008-10-09 2009-03-04 东华大学 Polyester based phase-change material having uvioresistant function and preparation thereof
CN104562292A (en) * 2014-12-29 2015-04-29 河南工程学院 Preparation method of porous micro-nano PET fibers
CN105019053A (en) * 2015-07-03 2015-11-04 山西瑞赛格纺织科技有限公司 Weaving phase-change energy-storage polyester fiber

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付蕾 等: "采用DSC测量PEG10000熔融焓变测定条件的研究", 《塑料科技》 *
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108642599A (en) * 2018-04-24 2018-10-12 苏州龙杰特种纤维股份有限公司 A kind of phase change fiber and preparation method thereof
CN113393958A (en) * 2021-06-17 2021-09-14 山东大学 Transparent flexible electrode with ordered grid structure and preparation method and application thereof

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