CN114855290A - Intelligent temperature-regulating phase-change fiber and preparation method thereof - Google Patents
Intelligent temperature-regulating phase-change fiber and preparation method thereof Download PDFInfo
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- CN114855290A CN114855290A CN202210145054.1A CN202210145054A CN114855290A CN 114855290 A CN114855290 A CN 114855290A CN 202210145054 A CN202210145054 A CN 202210145054A CN 114855290 A CN114855290 A CN 114855290A
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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
- 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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- 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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/04—Blended or other yarns or threads containing components made from different materials
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
- D10B2201/01—Natural vegetable fibres
- D10B2201/02—Cotton
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2211/00—Protein-based fibres, e.g. animal fibres
- D10B2211/20—Protein-derived artificial fibres
- D10B2211/22—Fibroin
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/02—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyamides
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
- D10B2331/041—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET] derived from hydroxy-carboxylic acids, e.g. lactones
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 provides an intelligent temperature-regulating phase-change fiber, which comprises the following steps: (1) and (3) placing the phase-change microcapsules in a polyvinyl alcohol solution, performing ultrasonic dispersion, filtering and drying to obtain the polyvinyl alcohol-coated microcapsules. (2) Adding the polyvinyl alcohol microcapsules obtained in the step (1) into spinning polymer material slices, uniformly mixing, heating, melt spinning, drafting, passing nascent fibers through a sodium hydroxide aqueous solution, drafting, and rolling to obtain the intelligent temperature-regulating phase-change fibers. The fiber has good biocompatibility and simple preparation method, the obtained intelligent temperature-regulating phase-change fiber has higher phase-change enthalpy, the leakage of the phase-change material can be effectively prevented in the use process, and the obtained fiber has good softness and hand feeling.
Description
Technical Field
The invention belongs to the field of textile fiber materials, and particularly relates to an intelligent temperature-regulating phase-change fiber and a preparation method thereof.
Background
With the progress of textile science and technology, people have higher and higher requirements on the functionalization of textile materials, so that the research on fiber materials in the prior art gradually changes to the direction of functionalization and intellectualization. The smart fiber can endow the traditional fiber industry with higher added value, and the market demand of the smart fiber is also expanded year by year, so that the research on the smart fiber is further and deeply carried out by large families.
The intelligent temperature-adjusting phase-change fiber can realize the control of heat energy through the added substances in the fiber, form a tiny constant temperature environment and improve the comfort level of wearing the fiber. The intelligent temperature-regulating fiber is a functional fiber developed by mainly utilizing the characteristics of latent heat release or absorption and constant temperature in the phase change process of substances, and has a bidirectional automatic temperature-regulating function.
Phase Change Materials (PCM) refers to Materials that can undergo Phase transition at a relatively stable temperature and absorb or release a large amount of heat during the Phase transition. The key point in the preparation process of the intelligent temperature-regulating fiber is the selection of the phase-change material, and the phase-change material with the proper threshold temperature can be selected to regulate the regulated temperature.
The method mainly comprises three methods for preparing the phase-change fiber, wherein one method is spinning filling, the method is to prepare a hollow fiber through a special spinning nozzle, then fill a phase-change material into the hollow cavity, and then seal the two ends of the fiber, for example, the invention patent with the publication number of CN108570766A, which is applied by Guangzhou energy research institute of Chinese academy of sciences, discloses a method for preparing a phase-change heat storage fiber membrane with a core-shell structure by using a coaxial electrostatic spinning technology, and the method mainly comprises the steps of adding the phase-change material into a first solvent and stirring until the phase-change material is completely dissolved to obtain a core-layer solution; adding the high polymer material into a second solvent, and stirring until the high polymer material is completely dissolved to obtain a shell solution; and (3) respectively injecting the nuclear layer solution obtained in the step (1) and the shell layer solution obtained in the step (2) into two solution channels of a coaxial electrostatic spinning device, and adjusting parameters of the coaxial electrostatic spinning device to carry out electrostatic spinning to obtain the phase-change heat storage fiber membrane with the core-shell structure. The second method for preparing the phase-change fiber is a microcapsule method, which is a method of preparing a phase-change material into microcapsules and adding the microcapsules into a spinning solution, and is common in the prior art, and can prevent the phase-change material from overflowing, for example, the invention patent with the publication number of CN107268098A, which is applied by Donghua university and Hengtian biological materials engineering technology Limited, discloses a polymer/phase-change microcapsule composite fiber and a preparation method thereof, wherein the phase-change microcapsule is dispersed into a nitrogen oxide aqueous solution of nitrogen methylmorpholine with the concentration of 50 wt% to obtain a dispersion liquid, a polymer is added into the dispersion liquid, the mixture is stirred and mixed in a low vacuum state and then subjected to dehydration treatment to obtain a mixed dispersion liquid, then the mixture is stirred and dehydrated in a high vacuum state to obtain a functional spinning solution, and finally the polymer/phase-change microcapsule composite fiber is prepared by spinning. The third is a chemical copolymerization method: a method for preparing a high molecular polymer with solid-solid phase change material performance by linking groups with an energy storage function to a main chain or a side chain of the high molecular polymer by adopting a graft copolymerization and block copolymerization method, and then preparing a phase change fiber by adopting a single-screw extruder through a melt spinning method, for example, an invention patent with the publication number of CN101967697A applied by the university of Donghua discloses a preparation method of a biodegradable solid-solid phase change nanofiber or a biodegradable fiber membrane, which comprises the following steps: (1) firstly, sequentially adding a coupling agent and a catalyst into a water dispersion of cellulose nanocrystals, dropwise adding an ethanol solution containing a dehydrating agent, stirring and reacting for 6-10 hours to prepare a water dispersion of carboxylated cellulose nanocrystals; (2) sequentially adding PEG and a catalyst into the aqueous dispersion of the carboxylated cellulose nanocrystal, dropwise adding an ethanol solution containing a dehydrating agent, and stirring for reaction for 10-12 hours to obtain a graft copolymer of the polyethylene glycol grafted cellulose nanocrystal; (3) preparing the aqueous solution of the graft copolymer as spinning solution for spinning.
The invention mainly aims to provide improvement on the technical problems that the phase change fiber prepared by a microcapsule method in the prior art is easy to cause phase change material seepage and mechanical property change. Because in the process of preparing the fiber by the microcapsules, the microcapsules are added into the spinning solution, and in the process of solidification and forming, the microcapsules are further fixed in the fiber, but when the fiber is made into a fabric and worn in use, the situations of folding, extrusion and the like are inevitable, and then the microcapsules are easily damaged, so that the phase-change material seeps out, and the phase-change effect is reduced. Meanwhile, the phase change material has a form change under a high temperature condition, which causes the change, so that the requirement on the temperature is high in the processing process. In addition, because the properties of the microcapsules are different from those of the fiber base material, when the microcapsules are added to the fiber base material, the softness of the fiber is greatly affected. Based on the problems in the prior art, the invention aims to provide a solution for preparing a fiber material capable of avoiding damage of microcapsules and improving the softness and handfeel of fibers.
Disclosure of Invention
The invention aims to provide an intelligent temperature-regulating phase-change fiber and a preparation method thereof.
The invention provides an intelligent temperature-regulating phase-change fiber and a preparation method thereof, which are characterized by comprising the following steps:
(1) putting the phase-change microcapsules into a polyvinyl alcohol solution, performing ultrasonic dispersion, filtering and drying to obtain polyvinyl alcohol-coated microcapsules;
(2) adding the polyvinyl alcohol microcapsules obtained in the step (1) into spinning polymer material slices, uniformly mixing, heating, melt spinning, drafting, passing nascent fibers through a sodium hydroxide aqueous solution, drafting, and rolling to obtain the intelligent temperature-regulating phase-change fibers.
The core material in the phase change microcapsule in the step (1) is one or more of polyethylene glycol, paraffin, stearic acid, lauric acid, sebacic acid, polyethylene glycol monoacrylate, stearoyl chloride, lauroyl chloride and sebacoyl chloride.
The wall material in the phase change microcapsule in the step (1) is any one or a combination of at least two of methyl methacrylate, styrene, butyl methacrylate, butyl acrylate, hydroxyethyl methacrylate, acrylic acid, divinyl benzene and 1, 4-butanediol diacrylate.
The preparation method of the phase-change microcapsule in the step (1) comprises the steps of dissolving an emulsifier in water to obtain a solution I, and blending core material monomers and wall material monomers to obtain a solution II; and (3) dropwise adding the solution II into the solution I, shearing at a high speed to form stable emulsion, dropwise adding an initiator, reacting for a certain time, standing, performing suction filtration, washing, and drying to constant weight to obtain the phase-change microcapsule.
The initiator is any one of potassium persulfate, ammonium persulfate or sodium persulfate.
The emulsifier is one or two of OP-10, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfonate and span-60.
In the preparation method of the phase-change microcapsule in the step (1), the reaction temperature is 50-70 ℃.
The size of the microcapsule is less than 5 μm, and the size of the microcapsule coated by the polyvinyl alcohol is less than 10 μm.
The content of the core material accounts for 30-60%, preferably 40-50% of the total mass of the core material and the wall material.
The polymer material slices in the step (2) are polylactic acid.
The adding amount of the polyvinyl alcohol microcapsules in the step (2) is 1-10%.
The winding speed of the step (2) is 500-600 m/min.
The melt spinning temperature in the step (2) is 155-170 ℃, and the aperture of the spinneret plate is more than 40 mu m.
The concentration of the sodium hydroxide aqueous solution in the step (2) is 0.1-5 g/L.
In the invention, the polyvinyl alcohol solution is used as a coating substance of the microcapsule, so that a layer of soluble polyvinyl alcohol layer can be obtained on the surface layer of the microcapsule. Due to the volume change of the phase-change material and the difference of the heat resistance of the wall material, the poor heat resistance of the phase-change microcapsule generally has the defect that the heat resistance of the microcapsule is lower than 160 ℃. The heat resistance of the microcapsule can be improved by coating the polyvinyl alcohol layer, so that the microcapsule can be realized by melt spinning.
In consideration of the heat resistance of the phase-change microcapsule, the invention uses polylactic acid as a fiber base material, and the polylactic acid fiber can be obtained by drafting the polylactic acid at the spinning temperature of about 160 ℃, thereby avoiding the damage of the microcapsule.
The invention prepares the microcapsule by an emulsion polymerization method, and the method ensures that the prepared microcapsule has small size which is generally less than 5 mu m under the action of high-speed shearing force. The coating effect is excellent, the coated core material can reach 30-60%, the coating rate is high, and the temperature of the obtained phase change microcapsule is high.
Because the phase-change material of the microcapsule has volume change in the processes of heat absorption and heat dissipation, the microcapsule has certain shrinkage performance, but because the shrinkage performance of the fiber base material and the microcapsule is different, the microcapsule in the fiber can be extruded between the fiber base material and the microcapsule in the process of temperature adjustment, the leakage of the phase-change material is easily caused, and the hand feeling and the mechanical performance of the fiber are influenced. Based on the point, the invention adheres a polyvinyl alcohol layer on the surface layer of the microcapsule, in the process of melt spinning, the microcapsule coated by polyvinyl alcohol is fixed in the fiber, in the process of spinning and drafting, when the nascent fiber passes through the aqueous solution of sodium hydroxide, the polyvinyl alcohol is dissolved, so that the fiber is recorded between the microcapsules to generate a certain gap, in the process of heat absorption and heat release of the microcapsule, the extrusion between the microcapsules and the fiber can not be generated, and the hand feeling and the flexibility of the fiber can be further improved.
The invention also provides an intelligent temperature-regulating phase-change fiber, which comprises a fiber base material and phase-change microcapsules, wherein the fiber base material is polylactic acid, a certain gap is formed between the phase-change microcapsules and the fiber base material, and the heat storage capacity of the phase-change material microcapsules of the microcapsules is 110-150J/g.
The microcapsule prepared by the invention can be used as an independent finishing agent and can be used together with other finishing agents, the microcapsule can be added into fibers to endow the fibers with composite performance, for example, the microcapsule can be used with an inorganic formaldehyde absorbent remover, the inorganic formaldehyde remover is nano titanium dioxide, and the composite finishing agent can endow the fibers with phase change performance and formaldehyde removal function at the same time.
The invention provides a yarn prepared from the fibers, which is obtained by spinning or blending the phase-change fibers, wherein the blended yarn comprises one or more of other fibers such as terylene, cotton, nylon and silk.
The invention also provides a phase change fabric, which is prepared from the phase change yarn.
The intelligent temperature-regulating phase-change fiber prepared by the invention has good biocompatibility due to the fact that the base material is polylactic acid, the obtained fiber is simple in preparation method, the obtained intelligent temperature-regulating phase-change fiber has high phase-change enthalpy, the leakage of a phase-change material can be effectively prevented in the using process, and the obtained fiber is good in flexibility and hand feeling.
The fiber prepared by the invention also has good mechanical property, the yarn prepared by the fiber has good spinnability, and the fabric prepared by the yarn has good intelligent temperature control performance and can be widely applied to the field of intelligent temperature control clothing.
Drawings
FIG. 1: the preparation idea schematic diagram of the intelligent temperature-regulating phase-change fiber is disclosed;
FIG. 2: morphology of the microcapsules prepared in examples 1-2.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention will be further explained with reference to examples, which are not intended to limit the present invention in any way.
As shown in fig. 1, in order to prepare the idea of the present disclosure, a first step is to prepare a phase-change microcapsule, wherein a core material of the phase-change microcapsule is one or more of polyethylene glycol, paraffin, stearic acid, lauric acid, sebacic acid, polyethylene glycol monoacrylate, stearoyl chloride, lauroyl chloride, and sebacoyl chloride. The wall material in the phase change microcapsule is any one or the combination of at least two of methyl methacrylate, styrene, butyl methacrylate, butyl acrylate, hydroxyethyl methacrylate, acrylic acid, divinyl benzene and 1, 4-butanediol diacrylate.
And secondly, coating polyvinyl alcohol on the surface layer of the prepared phase change microcapsule to ensure that the microcapsule is a multilayer phase change microcapsule, and protecting the microcapsule to prevent the damage of the microcapsule in the subsequent release process.
And the third step is to add the phase-change microcapsules coated by the polyvinyl alcohol into the spinning solution for spinning, and the third schematic diagram shown in fig. 1 is the obtained nascent fiber, which is not solidified and formed, so that the phase-change microcapsules are still coated by the polyvinyl alcohol in the fiber.
And the fourth step is the subsequent steps of curing molding and the like, wherein during curing molding, due to the solubility of the polyvinyl alcohol, the polyvinyl alcohol can be separated out from the fibers, so that the phase-change microcapsules and the fiber main body paper form a gap, the microcapsules have a certain space, the handfeel of the fibers is further improved, and meanwhile, the gap can prevent the microcapsules from being extruded in the phase-change process and prevent the microcapsules from being damaged.
The specific preparation examples are as follows:
example 1
Preparation of phase-change microcapsules
Dissolving span-60 in water to obtain a solution I, wherein the using amount of the span-60 is 5g/L, and blending a core material monomer and a wall material monomer to obtain a solution II, wherein the core material is paraffin, the wall material is acrylate, and the mass ratio of the paraffin to the acrylate is 1: 0.8-1.2; and dropwise adding the solution II into the solution I, shearing at a high speed at a rotating speed of 3000r/min to form a stable emulsion, dropwise adding an initiator, reacting at a reaction temperature of 70 ℃ for 5 hours, standing, performing suction filtration, washing, and drying to constant weight to obtain the phase-change microcapsule.
Example 2
Preparation of phase-change microcapsules
Dissolving span-60 in water to obtain a solution I, wherein the using amount of the span-60 is 5g/L, and blending a core material monomer and a wall material monomer to obtain a solution II, wherein the core material is stearic acid, the wall material is acrylate, and the mass ratio of paraffin to the acrylate is 1: 0.8-1.2; and dropwise adding the solution II into the solution I, shearing at a high speed at a rotating speed of 3000r/min to form a stable emulsion, dropwise adding an initiator, reacting at a reaction temperature of 70 ℃ for 5 hours, standing, performing suction filtration, washing, and drying to constant weight to obtain the phase-change microcapsule.
Example 3
Polyvinyl alcohol coated phase-change microcapsule
The microcapsule prepared in example 1 was put into an aqueous solution of polyvinyl alcohol at a concentration of 5g/L, dispersed by ultrasound, filtered, and dried to obtain a polyvinyl alcohol-coated microcapsule.
Example 4
Polyvinyl alcohol coated phase-change microcapsule
The microcapsule prepared in example 2 was put into an aqueous solution of polyvinyl alcohol at a concentration of 5g/L, dispersed by ultrasonic, filtered, and dried to obtain a microcapsule coated with polyvinyl alcohol.
Example 5
Preparation of intelligent temperature-regulating phase-change fiber
Adding the polyvinyl alcohol microcapsules obtained in the embodiment 2 into polylactic acid slices, wherein the adding amount of the microcapsules accounts for 5% of polylactic acid, uniformly mixing, heating, carrying out melt spinning through a screw extruder at the spinning temperature of 160 ℃, the pore diameter of a spinneret plate is 75 microns, carrying out dry-jet wet spinning, passing nascent fibers through a sodium hydroxide aqueous solution at the concentration of 0.5g/L and the temperature of 50 ℃, drafting, rolling and rolling at the speed of 500m/min, and thus obtaining the intelligent temperature-regulating phase-change fibers.
Example 6
Preparation of intelligent temperature-regulating phase-change fiber
Adding the polyvinyl alcohol microcapsules obtained in the embodiment 4 into polylactic acid slices, wherein the adding amount of the microcapsules accounts for 5% of polylactic acid, uniformly mixing, heating, carrying out melt spinning through a screw extruder at the spinning temperature of 160 ℃, the pore diameter of a spinneret plate is 75 microns, carrying out dry-jet wet spinning, passing nascent fibers through a sodium hydroxide solution at the concentration of 0.5g/L and the temperature of 50 ℃, drafting, rolling and rolling at the speed of 500m/min to obtain the intelligent temperature-regulating phase-change fibers.
Example 7
Preparation of intelligent temperature-regulating phase-change fiber
Adding the polyvinyl alcohol microcapsules obtained in the embodiment 2 into polylactic acid slices, wherein the adding amount of the microcapsules accounts for 1% of polylactic acid, uniformly mixing, heating, carrying out melt spinning through a screw extruder at the spinning temperature of 160 ℃, the pore diameter of a spinneret plate is 75 microns, carrying out dry-jet wet spinning, passing nascent fibers through a sodium hydroxide aqueous solution at the concentration of 0.5g/L and the temperature of 50 ℃, drafting, rolling and rolling at the speed of 500m/min, and thus obtaining the intelligent temperature-regulating phase-change fibers.
Example 8
Preparation of intelligent temperature-regulating phase-change fiber
Adding the polyvinyl alcohol microcapsules obtained in the embodiment 2 into polylactic acid slices, wherein the adding amount of the microcapsules accounts for 10% of polylactic acid, uniformly mixing, heating, carrying out melt spinning through a screw extruder at the spinning temperature of 160 ℃, the pore diameter of a spinneret plate is 75 microns, carrying out dry-jet wet spinning, passing nascent fibers through a sodium hydroxide aqueous solution at the concentration of 0.5g/L and the temperature of 50 ℃, drafting, rolling and rolling at the speed of 500m/min, and thus obtaining the intelligent temperature-regulating phase-change fibers.
Example 9
Preparation of intelligent temperature-regulating phase-change fiber
Adding the polyvinyl alcohol microcapsules obtained in the embodiment 2 into polylactic acid slices, wherein the adding amount of the microcapsules accounts for 5% of polylactic acid, uniformly mixing, heating, carrying out melt spinning through a screw extruder at the spinning temperature of 160 ℃, the pore diameter of a spinneret plate is 75 microns, carrying out dry-jet wet spinning, passing nascent fibers through a sodium hydroxide aqueous solution at the concentration of 0.5g/L and the temperature of 50 ℃, drafting, rolling, and the rolling speed is 600m/min, so as to obtain the intelligent temperature-regulating phase-change fibers.
Comparative example 1
Preparation of intelligent temperature-regulating phase-change fiber
Adding the microcapsule obtained in the embodiment 1 into polylactic acid slices, wherein the adding amount of the microcapsule accounts for 5% of polylactic acid, uniformly mixing, heating, carrying out melt spinning by a screw extruder at the spinning temperature of 160 ℃ and the aperture of a spinneret plate of 75 mu m, carrying out dry-jet wet spinning, and carrying out primary fiber treatment on sodium hydroxide aqueous solution at the concentration of 0.5g/L and the temperature of 50 ℃, drafting, rolling and the rolling speed of 500m/min to obtain the intelligent temperature-regulating phase-change fiber.
When the microcapsules prepared in examples 1 to 2 were observed, as shown in fig. 2, it was found that the microcapsules prepared were regular in shape and consistent in capsule size.
Comparing the fibers prepared in examples 4 to 9 with those prepared in comparative example 1, and evaluating the softness of the fibers by touching, kneading and the like, it is apparent that the fibers prepared in comparative example 1 are relatively stiff and have relatively high hardness, while the fibers prepared in examples 4 to 9 have relatively soft hand, which is probably due to the fact that the polyvinyl alcohol on the upper surface layer of the microcapsules is fused during the curing process of the fibers, so that the inside of the fibers is called as a porous structure, and the softness of the fibers is improved.
Certain exemplary embodiments of the present disclosure have been described above by way of illustration only, and it is needless to say that the described embodiments may be modified in various ways by those skilled in the art without departing from the spirit and scope of the present disclosure. Accordingly, the drawings and description are illustrative in nature and should not be construed as limiting the scope of the disclosure.
Claims (9)
1. An intelligent temperature-regulating phase-change fiber and a preparation method thereof are characterized by comprising the following steps:
(1) putting the phase-change microcapsules into a polyvinyl alcohol solution, performing ultrasonic dispersion, filtering and drying to obtain polyvinyl alcohol-coated microcapsules;
(2) adding the polyvinyl alcohol microcapsules obtained in the step (1) into spinning polymer material slices, uniformly mixing, heating, melt spinning, drafting, passing nascent fibers through a sodium hydroxide aqueous solution, drafting, and rolling to obtain the intelligent temperature-regulating phase-change fibers.
2. The intelligent temperature-regulating phase-change fiber and the preparation method thereof according to claim 1, wherein the core material in the phase-change microcapsule of the step (1) is one or more of polyethylene glycol, paraffin, stearic acid, lauric acid, sebacic acid, polyethylene glycol monoacrylate, stearoyl chloride, lauroyl chloride and sebacoyl chloride.
3. The intelligent temperature-regulating phase-change fiber and the preparation method thereof according to claim 1, wherein the wall material in the phase-change microcapsules of step (1) is any one or a combination of at least two of methyl methacrylate, styrene, butyl methacrylate, butyl acrylate, hydroxyethyl methacrylate, acrylic acid, divinylbenzene and 1, 4-butanediol diacrylate.
4. The intelligent temperature-regulating phase-change fiber and the preparation method thereof according to claim 1, wherein the phase-change microcapsule of the step (1) is prepared by dissolving an emulsifier in water to obtain a solution I, and blending the core material monomer and the wall material monomer to obtain a solution II; and (3) dropwise adding the solution II into the solution I, shearing at a high speed to form stable emulsion, dropwise adding an initiator, reacting for a certain time, standing, performing suction filtration, washing, and drying to constant weight to obtain the phase-change microcapsule.
5. The intelligent temperature-regulating phase-change fiber as claimed in claim 4, and the preparation method thereof, is characterized in that: the initiator is any one of potassium persulfate, ammonium persulfate or sodium persulfate; the emulsifier is one or two of OP-10, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfonate and span-60, the reaction temperature in the preparation method of the phase-change microcapsule is 50-80 ℃, the size of the microcapsule is less than 5 mu m, and the size of the microcapsule coated by the polyvinyl alcohol is less than 10 mu m; the content of the core material accounts for 30-60%, preferably 40-50% of the total mass of the core material and the wall material.
6. The intelligent temperature-regulating phase-change fiber and the preparation method thereof according to claim 1, wherein the polymer material slices in the step (2) are polylactic acid; the adding amount of the polyvinyl alcohol microcapsules in the step (2) is 1-10%; the winding speed of the step (2) is 500-600 m/min; the melt spinning temperature in the step (2) is 155-170 ℃, and the aperture of a spinneret plate is more than 40 mu m; the concentration of the sodium hydroxide aqueous solution in the step (2) is 0.1-5 g/L.
7. The intelligent temperature-regulating phase-change fiber and the fiber obtained by the preparation method thereof according to any one of claims 1 to 6, wherein the fiber comprises a fiber base material and phase-change microcapsules, the fiber base material is polylactic acid, a certain gap is formed between the phase-change microcapsules and the fiber base material, and the heat storage capacity of the phase-change material microcapsules of the microcapsules is 110-150J/g.
8. A phase change yarn prepared by using the fiber of claim 7, wherein the phase change yarn is obtained by spinning or blending the phase change fiber, and the blended yarn comprises one or more of terylene, cotton, nylon and silk as other fibers.
9. A phase change fabric produced using the phase change yarn of claim 9, the phase change fabric being produced from the phase change yarn.
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| US20130273365A1 (en) * | 2001-09-21 | 2013-10-17 | Mark H. Hartmann | Cellulosic Fibers Having Enhanced Reversible Thermal Properties and Methods of Forming Thereof |
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