CN115198387A - Preparation method of emulsion electrostatic spinning skin-core structure phase-change fiber - Google Patents

Preparation method of emulsion electrostatic spinning skin-core structure phase-change fiber Download PDF

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Publication number
CN115198387A
CN115198387A CN202210620067.XA CN202210620067A CN115198387A CN 115198387 A CN115198387 A CN 115198387A CN 202210620067 A CN202210620067 A CN 202210620067A CN 115198387 A CN115198387 A CN 115198387A
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China
Prior art keywords
spinning
phase
water
stirring
change
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CN202210620067.XA
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Chinese (zh)
Inventor
权震震
许钰青
杨卫国
杨燿斌
卫国
覃小红
俞建勇
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Donghua University
Bros Eastern Co Ltd
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Donghua University
Bros Eastern Co Ltd
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Priority to CN202210620067.XA priority Critical patent/CN115198387A/en
Publication of CN115198387A publication Critical patent/CN115198387A/en
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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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
    • 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
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • 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
    • D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30—Conjugate filaments; Spinnerette packs therefor
    • D01D5/34—Core-skin structure; Spinnerette packs therefor
    • 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
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The invention relates to a preparation method of emulsion electrostatic spinning skin-core structure phase-change fibers. The method comprises the following steps: dissolving a water-soluble polymer in water, and stirring to obtain a polymer aqueous solution; dissolving an emulsifier in water, adding a phase-change material, and stirring to obtain a spinning emulsion precursor; and mixing the polymer aqueous solution with the spinning emulsion precursor, stirring to obtain spinning emulsion, and carrying out electrostatic spinning and drying. The method adopts the single-needle spinneret device to prepare the skin-core structure phase-change fiber, greatly simplifies the preparation device of the skin-core structure phase-change fiber, enhances the controllability of electrostatic spinning jet flow, obviously improves the anti-leakage performance of the electrostatic spinning phase-change fiber, and effectively solves the technical problem that the phase-change components in the phase-change temperature-adjusting textile are easy to leak.

Description

Preparation method of emulsion electrostatic spinning skin-core structure phase-change fiber
Technical Field
The invention belongs to the field of textile processing, and particularly relates to a preparation method of emulsion electrostatic spinning skin-core structure phase-change fibers.
Background
The Phase Change Material (PCM) is a novel energy storage material, and can be added into textiles to enable the 'microenvironment' between the textiles and a human body to be in an appropriate temperature range through phase transition so as to maintain the thermal comfort of the human body. Common existing forms of phase change materials in textiles include phase change microcapsules and phase change fibers, wherein the phase change microcapsules are often added into the textiles in a coating mode in a post-treatment process, however, the textiles obtained by the method often have the problems of low softness, poor air permeability and the like, and in contrast, the phase change fibers do not have great influence on inherent performance and subsequent processing of the textiles, so that the phase change fibers are widely applied.
In the phase change field, electrostatic spinning is used as an advanced means for manufacturing phase change fibers, compared with a common phase change fiber preparation method, the phase change fibers obtained by electrostatic spinning are mostly in a nanometer scale, have stable fiber appearance and larger specific surface area, and have better shape stability and larger temperature transmission area as a support material of a phase change component and higher thermal response speed. At present, the common electrostatic spinning equipment for preparing the phase-change fiber comprises uniaxial electrostatic spinning and coaxial electrostatic spinning, but the uniaxial electrostatic spinning and the coaxial electrostatic spinning both have obvious defects. The uniaxial electrostatic spinning has the advantages of simple jet flow stability, high phase change component content, low limitation on spinning temperature and controllable phase change component content, but when the spinning solution is in a solution state, the obtained fiber has the problems that the phase change material is not completely coated, namely the phase change material cannot be completely encapsulated, the liquid leakage phenomenon is easy to occur in the solid-liquid conversion process and the like, so that the application of some insoluble phase change materials is seriously limited, the coaxial electrostatic spinning can effectively solve the problem, the immiscible high polymer and the phase change material are respectively used as a skin layer and a core layer to prepare the skin-core structure phase change fiber, the liquid leakage problem of the materials in the solid-liquid phase change process is further solved, but the coaxial electrostatic spinning has higher requirements on equipment, the preparation process is complex, and the defects of low phase change material content in the fiber, unstable spinning jet flow, poor controllability and the like exist.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of emulsion electrostatic spinning skin-core structure phase-change fibers, so as to overcome the defects caused by adopting single-shaft electrostatic spinning or coaxial electrostatic spinning to prepare the phase-change fibers in the prior art. The invention adopts emulsion electrostatic spinning to disperse insoluble phase change substances in a polymer carrier which is easy to form fibers through emulsification so as to form uniform spinning emulsion, the required device is simple and convenient, the fiber with a sheath-core structure can be directly prepared only by adopting a single-shaft spinneret, the good encapsulation of the core layer phase change material in the sheath layer supporting material is realized, the defects of the single-shaft electrostatic spinning and the coaxial electrostatic spinning are perfectly overcome, and a new method is provided for preparing the phase change fiber.
The invention provides a preparation method of emulsion electrostatic spinning skin-core structure phase-change fiber, which comprises the following steps:
(1) Dissolving a water-soluble polymer in water, and stirring to obtain a polymer aqueous solution;
(2) Dissolving an emulsifier in water, adding a phase-change material, and stirring to obtain a spinning emulsion precursor;
(3) And (3) mixing the aqueous solution of the polymer obtained in the step (1) with the precursor of the spinning emulsion obtained in the step (2), stirring to obtain a spinning emulsion, and carrying out electrostatic spinning and drying to obtain the skin-core structure phase-change fiber.
Preferably, the water-soluble polymer in the step (1) is polyvinyl alcohol PVA.
More preferably, the polyvinyl alcohol PVA is polyvinyl alcohol PVA1788.
Preferably, the water-soluble polymer in the step (1) accounts for 10-12wt% of the total mass of the water-soluble polymer and the water in the step (1) and the step (2).
Preferably, the stirring temperature in the step (1) is 80-95 ℃, the stirring time is 2-3 h, and the stirring speed is 300-500 r/min.
Preferably, the emulsifier in step (2) is Sodium Dodecyl Benzene Sulfonate (SDBS).
Preferably, the phase change material in the step (2) is dodecanol DD or tetradecanol TD.
Preferably, the emulsifier in the step (2) accounts for 0.5-2wt% of the total mass of the water-soluble polymer in the step (1) and the water in the step (1) and the step (2); the phase-change material accounts for 5-10 wt% of the total mass of the water-soluble polymer in the step (1) and the water in the step (1) and the step (2).
Preferably, in the step (2), the stirring temperature is 70-85 ℃, the stirring time is 30-40 min, and the stirring speed is 800-1500 r/min.
Preferably, the mass ratio of the polymer aqueous solution to the spinning emulsion precursor in the step (3) is 1.47:1 to 1.77:1.
preferably, in the step (3), the stirring temperature is 70-85 ℃, the stirring time is 1-1.5 h, and the stirring speed is 800-1500 r/min.
Preferably, the process parameters of the electrostatic spinning in the step (3) are as follows: the extrusion amount of the spinning solution is 0.5ml/h-0.7ml/h, the spinning distance is 15cm-18cm, the spinning voltage is 15kV-18kV, the environmental temperature is set to be 24-28 ℃, the relative humidity is 40% -60%, the spinning time is 2-5h, and aluminum foil is adopted for receiving.
Preferably, the drying in the step (3) is silica gel drying.
The invention also provides the skin-core structure phase-change fiber prepared by the preparation method.
The invention also provides an application of the skin-core structure phase-change fiber in textiles.
Advantageous effects
The invention adopts the single-needle spinneret device to prepare the skin-core structure phase-change fiber, greatly simplifies the preparation device of the skin-core structure phase-change fiber, enhances the controllability of electrostatic spinning jet flow, obviously improves the anti-leakage performance of the electrostatic spinning phase-change fiber, and effectively solves the technical problem that phase-change components in a phase-change temperature-adjusting textile are easy to leak.
Drawings
FIG. 1 is an SEM image of a skin-core structure phase-change fiber prepared by emulsion electrospinning in example 1.
FIG. 2 is a TEM image of the phase-change fiber with a sheath-core structure prepared by emulsion electrospinning in example 1.
FIG. 3 is a DSC curve of the phase change fiber with a sheath-core structure prepared by the emulsion electrospinning in example 1 after 15 thermal cycles.
FIG. 4 is a DSC curve of the phase-change fiber with a sheath-core structure prepared by the electrostatic spinning of the emulsion in example 3 after 15 thermal cycles.
FIG. 5 is a DSC curve of the phase-change fiber with a sheath-core structure prepared by the electrostatic spinning of the emulsion in example 4 after 15 thermal cycles.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the claims appended to the present application.
In all the following examples, PVA1788 was obtained from Allantin reagent (Shanghai) Co., ltd., and SDBS and DD were obtained from Shanghai pharmaceutical group chemical reagent Co., ltd. The mass fractions of all the chemicals were relative to the mass fraction of PVA in step (1) and the total ultrapure water in step (1) and step (2).
In all examples, the testing method and conditions for the anti-leakage performance are as follows: placing a 4mg phase-change fiber sample in a DSC8500 differential scanning calorimeter, setting the atmosphere as nitrogen, and the temperature rising and falling rate as 10 ℃/min to obtain a DSC curve of the sample which is circulated for 15 times at the temperature rising and falling of 0-50 ℃. And (4) analyzing the curve by using Pyris Manager software to obtain enthalpy values of the samples and enthalpy loss rate data before and after 15 times of heat cycles.
Example 1
(1) 10wt% (relative to PVA + H) 2 O, same as below) was dissolved in ultrapure water, and magnetically stirred at a rate of 500r/min for 3 hours under heating in a water bath at 90 ℃ to obtain an aqueous PVA solution.
(2) Dissolving 1wt% of sodium dodecyl benzene sulfonate SDBS in 10g of ultrapure water, adding 5wt% of dodecanol DD, and magnetically stirring for 40min at the speed of 1000r/min under the water bath heating condition of 80 ℃ to obtain a spinning emulsion precursor.
(3) Mixing the polyvinyl alcohol aqueous solution obtained in the step (1) and the spinning emulsion precursor obtained in the step (2) while the mixture is hot, wherein the mass ratio of the polyvinyl alcohol aqueous solution to the spinning emulsion precursor is 100.
(4) And (3) carrying out electrostatic spinning on the spinning emulsion, wherein the spinning temperature is 28 ℃, the relative humidity is 40%, the model of a spinning needle is 18 (the inner diameter is 0.86mm, the outer diameter is 1.26 mm), the extrusion capacity of the spinning solution is 0.5ml/h, the spinning distance is 16cm, and the spinning voltage is 15kV. And spinning for about 2 hours, receiving the obtained fiber by using an aluminum foil, and drying the silica gel to obtain the emulsion electrostatic spinning skin-core structure phase change fiber.
FIG. 1 shows that: the skin-core structure phase change fiber prepared by using dodecanol DD as a disperse phase, polyvinyl alcohol PVA as a continuous phase and sodium dodecyl benzene sulfonate SDBS as an emulsifier has good surface appearance.
FIG. 2 shows that: the prepared phase-change fiber has a uniform, continuous and well-defined skin-core structure inside, and the phase-change fiber is prepared by taking dodecanol DD as a disperse phase, polyvinyl alcohol PVA as a continuous phase and sodium dodecyl benzene sulfonate SDBS as an emulsifier.
FIG. 3 shows: after 15 times of thermal cycles, the enthalpy value of the phase-change fiber is changed from 33.8J/g to 33.7J/g, and the enthalpy loss rate is only 0.3 percent, thereby fully proving that the prepared skin-core structure phase-change fiber has good anti-leakage performance.
Example 2
(1) 12wt% (relative to PVA + H) 2 O, same as below) was dissolved in ultrapure water, and magnetically stirred at a rate of 500r/min for 3 hours under heating in a water bath at 90 ℃ to obtain an aqueous PVA solution.
(2) Dissolving 1wt% of sodium dodecyl benzene sulfonate SDBS in 10g of ultrapure water, adding 5wt% of dodecanol DD, and magnetically stirring for 40min at the speed of 1000r/min under the water bath heating condition of 80 ℃ to obtain a spinning emulsion precursor.
(3) Mixing the polyvinyl alcohol aqueous solution in the step (1) and the spinning emulsion precursor in the step (2) while the polyvinyl alcohol aqueous solution and the spinning emulsion precursor are hot, wherein the mass ratio of the polyvinyl alcohol aqueous solution to the spinning emulsion precursor is 103.
(4) And (2) carrying out electrostatic spinning on the spinning emulsion, wherein the spinning temperature is 28 ℃, the relative humidity is 40%, the type of a spinning needle head is 18 (the inner diameter is 0.86mm, the outer diameter is 1.26 mm), the extrusion amount of a spinning solution is 0.5ml/h, the spinning distance is 16cm, and the spinning voltage is 15kV. The spinning time is about 2h, the obtained fiber is received by aluminum foil, and the emulsion electrostatic spinning skin-core structure phase change fiber is obtained after silica gel drying.
Example 3
(1) 10wt% (relative to PVA + H) 2 O, same as below) was dissolved in ultrapure water, and magnetically stirred at a rate of 500r/min for 3 hours under heating in a water bath at 90 ℃ to obtain an aqueous PVA solution.
(2) Dissolving 1wt% of sodium dodecyl benzene sulfonate SDBS in 10g of ultrapure water, adding 8wt% of dodecanol DD, and magnetically stirring for 40min at the speed of 1000r/min under the water bath heating condition of 80 ℃ to obtain a spinning emulsion precursor.
(3) And (3) mixing the polyvinyl alcohol aqueous solution obtained in the step (1) and the spinning emulsion precursor obtained in the step (2) while the polyvinyl alcohol aqueous solution and the spinning emulsion precursor are hot, wherein the mass ratio of the polyvinyl alcohol aqueous solution to the spinning emulsion precursor is 200.
(4) And (3) carrying out electrostatic spinning on the spinning emulsion, wherein the spinning temperature is 28 ℃, the relative humidity is 40%, the model of a spinning needle is 18 (the inner diameter is 0.86mm, the outer diameter is 1.26 mm), the extrusion capacity of the spinning solution is 0.5ml/h, the spinning distance is 16cm, and the spinning voltage is 15kV. And spinning for about 2 hours, receiving the obtained fiber by using an aluminum foil, and drying the silica gel to obtain the emulsion electrostatic spinning skin-core structure phase change fiber.
FIG. 4 shows that: after 15 times of thermal cycles, the enthalpy value of the phase-change fiber is changed from 67.0J/g to 66.8J/g, and the enthalpy loss rate is only 0.3%, thereby fully proving that the prepared skin-core structure phase-change fiber has good anti-seepage performance.
Example 4
(1) 10wt% (relative to PVA + H) 2 O, same as below) was dissolved in ultrapure water, and magnetically stirred at a rate of 500r/min for 3 hours under heating in a water bath at 90 ℃ to obtain an aqueous PVA solution.
(2) Dissolving 1wt% of sodium dodecyl benzene sulfonate SDBS in 10g of ultrapure water, adding 10wt% of dodecanol DD, and magnetically stirring at the speed of 1000r/min for 40min under the water bath heating condition of 80 ℃ to obtain a spinning emulsion precursor.
(3) Mixing the polyvinyl alcohol aqueous solution obtained in the step (1) and the spinning emulsion precursor obtained in the step (2) while the mixture is hot, wherein the mass ratio of the polyvinyl alcohol aqueous solution to the spinning emulsion precursor is 200.
(4) And (2) carrying out electrostatic spinning on the spinning emulsion, wherein the spinning temperature is 28 ℃, the relative humidity is 40%, the type of a spinning needle head is 18 (the inner diameter is 0.86mm, the outer diameter is 1.26 mm), the extrusion amount of a spinning solution is 0.5ml/h, the spinning distance is 16cm, and the spinning voltage is 15kV. And spinning for about 2 hours, receiving the obtained fiber by using an aluminum foil, and drying the silica gel to obtain the emulsion electrostatic spinning skin-core structure phase change fiber.
FIG. 5 shows that: after 15 times of thermal cycles, the enthalpy value of the phase-change fiber is changed from 71.5J/g to 71.2J/g, and the enthalpy loss rate is only 0.42 percent, thereby fully proving that the prepared skin-core structure phase-change fiber has good anti-leakage performance.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention.

Claims (10)

1. A preparation method of emulsion electrostatic spinning skin-core structure phase-change fibers comprises the following steps:
(1) Dissolving a water-soluble polymer in water, and stirring to obtain a polymer aqueous solution;
(2) Dissolving an emulsifier in water, adding a phase-change material, and stirring to obtain a spinning emulsion precursor;
(3) And (3) mixing the polymer aqueous solution obtained in the step (1) with the spinning emulsion precursor obtained in the step (2), stirring to obtain a spinning emulsion, and carrying out electrostatic spinning and drying to obtain the skin-core structure phase-change fiber.
2. The method according to claim 1, wherein the water-soluble polymer in the step (1) is polyvinyl alcohol PVA; the water-soluble polymer accounts for 10-12wt% of the total mass of the water-soluble polymer and the water in the step (1) and the step (2).
3. The preparation method according to claim 1, characterized in that the stirring temperature in the step (1) is 80-95 ℃, the stirring time is 2-3 h, and the stirring speed is 300-500 r/min.
4. The method according to claim 1, wherein the emulsifier in step (2) is sodium dodecylbenzenesulfonate SDBS; the phase change material is dodecanol DD or tetradecanol TD.
5. The method according to claim 1, wherein the emulsifier in step (2) accounts for 0.5-2wt% of the total mass of the water-soluble polymer in step (1) and the water in step (1) and step (2); the phase-change material accounts for 5-10 wt% of the total mass of the water-soluble polymer in the step (1) and the water in the step (1) and the step (2).
6. The preparation method according to claim 1, wherein the stirring temperature in the step (2) is 70-85 ℃, the stirring time is 30-40 min, and the stirring speed is 800-1500 r/min.
7. The method according to claim 1, wherein the mass ratio of the aqueous polymer solution to the spinning emulsion precursor in the step (3) is 1.47:1 to 1.77:1; the stirring temperature is 70-85 ℃, the stirring time is 1-1.5 h, and the stirring speed is 800-1500 r/min.
8. The preparation method according to claim 1, wherein the electrostatic spinning in the step (3) has the following process parameters: the extrusion amount of the spinning solution is 0.5ml/h-0.7ml/h, the spinning distance is 15cm-18cm, the spinning voltage is 15kV-18kV, the environmental temperature is set to be 24-28 ℃, the relative humidity is 40% -60%, and the spinning time is 2-5h.
9. A core-sheath phase-change fiber prepared by the method of claim 1.
10. Use of the core-sheath phase change fiber according to claim 9 in textiles.
CN202210620067.XA 2022-06-02 2022-06-02 Preparation method of emulsion electrostatic spinning skin-core structure phase-change fiber Pending CN115198387A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103243407A (en) * 2013-05-16 2013-08-14 东华大学 Method for preparing skin-core structured drug-loading nanofiber through needleless electrostatic spinning technology
CN109576823A (en) * 2018-11-08 2019-04-05 华南理工大学 A kind of phase-changing energy storage material and preparation method thereof with core-skin fibre structure

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103243407A (en) * 2013-05-16 2013-08-14 东华大学 Method for preparing skin-core structured drug-loading nanofiber through needleless electrostatic spinning technology
CN109576823A (en) * 2018-11-08 2019-04-05 华南理工大学 A kind of phase-changing energy storage material and preparation method thereof with core-skin fibre structure

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
权震震 等: "乳液静电纺十二醇聚乙烯醇相变纤维性能研究", 《棉纺织技术》 *

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