CN111455483A - Radiation refrigeration fiber and preparation method of fabric thereof - Google Patents

Radiation refrigeration fiber and preparation method of fabric thereof Download PDF

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Publication number
CN111455483A
CN111455483A CN202010261960.9A CN202010261960A CN111455483A CN 111455483 A CN111455483 A CN 111455483A CN 202010261960 A CN202010261960 A CN 202010261960A CN 111455483 A CN111455483 A CN 111455483A
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fiber
radiation
nano particles
master batch
radiation refrigeration
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Inventor
陶光明
马耀光
曾少宁
马肖
吴嘉威
向远卓
吴鹏飞
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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Priority to CN202010261960.9A priority Critical patent/CN111455483A/en
Publication of CN111455483A publication Critical patent/CN111455483A/en
Priority to PCT/CN2021/078388 priority patent/WO2021203867A1/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
    • 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
    • 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
    • D01F6/46—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 polyolefins
    • 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
    • D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • 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
    • D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
    • 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
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04B—KNITTING
    • D04B1/00—Weft knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
    • D04B1/14—Other fabrics or articles characterised primarily by the use of particular thread materials
    • D04B1/16—Other fabrics or articles characterised primarily by the use of particular thread materials synthetic threads
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04B—KNITTING
    • D04B21/00—Warp knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Multicomponent Fibers (AREA)

Abstract

A method for preparing radiation refrigeration fiber and fabric thereof comprises the following steps: mixing the inorganic micro-nano particles and the polymer substrate material according to a preset weight ratio to prepare a composite material master batch; and carrying out composite extrusion molding on the composite master batch in a spinning assembly, and winding to obtain the radiation refrigeration fiber. According to the invention, high-concentration inorganic micro-nano particles are introduced into polymer fibers by using a melt composite spinning method, and the size of the micro-nano particles and the internal composite structure of the fibers are accurately regulated, so that the fibers have excellent daytime radiation refrigeration performance, high mechanical strength and high weaving performance, and the radiation refrigeration fabric suitable for cooling the surface of human skin is obtained, and has the advantages of large-scale batch preparation, low cost and high production efficiency.

Description

Radiation refrigeration fiber and preparation method of fabric thereof
Technical Field
The invention relates to the field of radiation refrigeration, in particular to a radiation refrigeration fiber and a preparation method of a fabric thereof.
Background
Energy is an important basis for human survival, and promotes the development and progress of society. The huge energy consumption causes economic loss and also brings excessive emission of greenhouse gases, which causes severe climate problems, and extreme weather such as high temperature is more severe and frequent. The resulting space heating and cooling requirements are now a major part of residential and commercial energy consumption, and constitute a significant challenge to human sustainable development. Face enormous energy consumption and health and economic threats brought by high temperature. Personal thermal management, a technology that provides heating or cooling only to an individual and its local environment, is becoming an increasingly effective solution for personalization. The passive thermal regulation performance is realized, meanwhile, the dependence of human on low-energy-efficiency cooling methods such as an air conditioner is reduced, the cooling cost of the whole building is effectively reduced, and the individual thermal comfort requirements are met more economically in an energy-saving manner.
With the rapid development of refrigeration technology, zero-energy-consumption radiation refrigeration technology based on intelligent cooling materials is produced. The radiation refrigeration technology realizes high reflectivity of an object in the wavelength range of solar radiation (0.3-2.5 microns) through material selection and structure design, and greatly blocks heat input of a human body through the solar radiation. Meanwhile, by utilizing a material with high emissivity or transparency in a human body radiation wave band, self heat is discharged to the outer space with the temperature close to absolute zero through an 'atmospheric window' in the form of electromagnetic waves, the purpose of self cooling is achieved, and zero energy consumption cooling is effectively realized. Although radiation refrigeration has become a research focus, the prior art methods have certain limitations to be applied to body cooling fabrics.
The university of Columbia Yuan Yang professor team, U.S. based on the phase reversal method, prepared a graded porous polymer coating with 5 μm micropores and 50nm-500nm nanopores for radiation refrigeration using a P (VdF-HFP)/acetone/water mixed solution. Because the micro-nano holes can effectively scatter solar radiation, and the P (VdF-HFP) coating can effectively radiate heat by a plurality of absorption peaks within the range of 8-13 mu m, the coating with the thickness of about 300 mu m realizes 96% of high solar reflectivity and 97% of high thermal emissivity, and the temperature can be reduced by about 6 ℃ by testing the refrigeration performance of passive radiation under sunlight to generate about 96Wm-2Cooling power of (2).
Another radiation refrigeration coating, as disclosed in chinese patent CN 110628325 a, comprises a reflection heat insulation layer and a top protection layer, the reflection heat insulation layer is composed of a high temperature resistant base material, a high temperature resistant radiation refrigeration pigment and other additives, the protection layer comprises titanium dioxide sol and silica sol, the coating prepared by the invention has a reflectivity of more than 80% for visible light and infrared light, an infrared emissivity of more than 80% in an atmospheric window waveband, and a blocking effect for ultraviolet rays, and can be used for a long time in an environment with a temperature of-40 ℃ to 500 ℃. Although the coating material has radiation refrigeration performance and can provide heat dissipation and ultraviolet resistance protection effects for objects, the coating material does not have wearability and cannot be used for local cooling of human bodies.
A team at the university of Colorado, USA, prepared a random glass-polymer mixed metamaterial, in which a random distribution resonance dielectric SiO is embedded in a transparent polymer methyl pentene2Microspheres and a silver film as a backing, the 50-micron-thick metamaterial prepared by using the silver film as the backing can reflect about 96% of solar radiation, has high emissivity of more than 93% between 8 and 13 microns and can generate more than 100W m in direct sunlight-2The radiant cooling power of. Film(s)The radiation refrigeration material in the state is also applied to production and life as disclosed in Chinese patent CN 109968769A, micron particles and polymer solution are mixed, a film is prepared in an extrusion mode to be used as a sunlight reflecting layer, a micro-nano powder and fluorescent agent mixture is sprayed to prepare an ultraviolet absorption fluorescent rough layer, the average solar energy reflectivity of the film prepared by the method reaches 97%, and the average radiation rate of an atmospheric window reaches 95%. However, the method has complex steps, cannot be formed in one step, and the prepared film has poor flexibility, cannot be used for cooling the human body and is only suitable for the industrial field. The other polymer radiation refrigeration film added with the titanium dioxide hollow spheres, such as Chinese patent CN109705819A, is prepared by uniformly mixing the titanium dioxide hollow spheres with a copolymer of vinylidene fluoride and hexafluoropropylene and coating the mixture, so that the high emissivity in the range of 8-13 mu m and the high reflectivity of a solar radiation wave band are realized. Although the above film material has effective cooling radiation refrigeration performance, it lacks air permeability and comfort, and the method cannot be mass-produced, and is not suitable for cooling human body.
Compared with the film-state, fibrous radiation refrigeration material, such as that disclosed in chinese patent CN110042564A, the material has the characteristics of air and moisture permeability and flexibility more suitable for human body heat management, and has good monodispersity and high emission of radiation particles SiO2The microspheres are uniformly dispersed in a polymer, such as PE, PA6, PMMA and PVDF solution, and a fiber film is obtained through electrostatic spinning, so that the fiber film has the capability of cooling the surface of human skin by radiation.
The melt spinning method can realize the rapid preparation of mass fibers, and has simple process and high production efficiency. For example, chinese patent CN102677218A, the uvioresistant polyphenylene sulfide fiber prepared by the melt spinning method contains 90% to 99.9% of polyphenylene sulfide resin and 0.01% to 10% of light stabilizer, and has higher ultraviolet light stability and light stability lasting time. For example, as disclosed in CN103668538B, the biomass polyester fiber with anti-uv effect can be prepared by melt spinning the anti-uv master batch, such as 1% -5% of nano titanium dioxide, 1% -5% of nano titanium nitride, and biomass polyester chip. However, the fiber prepared by the melt spinning method has the function of ultraviolet resistance, cannot regulate solar radiation and human body heat radiation, and cannot be used for personal heat management.
Chinese patent CN110685031A discloses that a melt spinning method is used to melt and spin functional filler with the grain diameter of 1-20 μm and the mass fraction of 1-17%, such as SiO2、SiC、TiO2、CaCO3、BaSO4、Si3N4、ZnO、Al2O3、Fe2O3、ZrO2Or jade powder, and a base material, such as polypropylene, polyvinyl alcohol, polyvinyl chloride, polyurethane, polyester, polyethylene, polyamide, polymethyl methacrylate, polyvinylidene fluoride or polyacrylonitrile, are mixed to prepare the radiation refrigeration fiber, the radiation refrigeration fabric obtained by further weaving has a reflectivity of more than 60% to a solar radiation waveband, has an emissivity of more than 80% to a human body thermal radiation waveband, and a good cooling effect can be used for preparing textiles with cooling requirements. However, the method cannot accurately regulate the particle size range of the functional filler, the mass fraction of the functional filler doped in the fiber is low, and the reflectivity in a solar radiation waveband is low, so that the daytime radiation performance is poor; on the other hand, the invention can not realize the structural control of the interior of the fiber, and can limit the radiation refrigeration effect and the mechanical property of the fiber.
In summary, the existing radiation refrigeration material has the following disadvantages: (1) most of the materials are in a coating or film state, and the materials are not enough in air permeability and comfort and cannot be used for cooling human skin; (2) the methods such as electrostatic spinning and the like have complex process and high cost; (3) the composite fiber prepared by the existing melt spinning method has poor daytime radiation refrigeration effect. Therefore, a technology for preparing radiation refrigeration fibers by introducing high-concentration inorganic micro-nano particles by using a melt composite spinning method is lacked, and the fibers have excellent radiation refrigeration performance and high mechanical strength and knittability by accurately regulating and controlling the size of the micro-nano particles and the internal composite structure of the fibers, so that high-comfort fabrics suitable for cooling human skins are prepared, large-scale batch preparation is realized, and the advantages of low cost and high production efficiency are achieved.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a batch preparation method for radiation refrigeration fibers and fabrics thereof, which can introduce high-concentration micro-nano particles by using melt composite spinning, and can accurately regulate and control the size and fiber structure of the micro-nano particles.
In order to solve the above problems, the present invention mainly provides the following technical solutions:
a method of making a radiation-cooled fiber, comprising:
mixing the inorganic micro-nano particles and the polymer substrate material according to a preset weight ratio to prepare a composite material master batch;
and carrying out composite extrusion molding on the composite master batch in a spinning assembly, and winding to obtain the radiation refrigeration fiber.
Preferably, the inorganic micro-nano particles and the polymer substrate material are mixed according to a predetermined weight ratio to prepare the composite material master batch, which comprises,
uniformly mixing first inorganic micro-nano particles and a first polymer base material according to a preset first weight ratio to prepare a first composite material master batch, and uniformly mixing second inorganic micro-nano particles and a second polymer base material according to a preset second weight ratio to prepare a second composite material master batch;
the method comprises the steps of taking the first composite material master batch as a first component and the second composite material master batch as a second component, carrying out composite extrusion molding in the spinning assembly, and winding to obtain the radiation refrigeration fiber.
Preferably, the weight ratio of the inorganic micro-nano particles in the first composite material master batch is 1-80%, the weight ratio of the inorganic micro-nano particles in the second composite material master batch is 0-20%, and the weight ratio of the inorganic micro-nano particles in the first composite material master batch is more than or equal to the weight ratio of the inorganic micro-nano particles in the second composite material master batch.
Preferably, the first polymer substrate material and the second polymer substrate material may be the same or different; the first inorganic micro-nano particles and the second inorganic micro-nano particles can be the same or different.
Preferably, the radiation refrigeration fiber further comprises at least one third component, wherein the at least one third component, the first component and the second component are subjected to composite extrusion molding in a spinning assembly, and the radiation refrigeration fiber is obtained after winding;
the at least one third component is at least one third composite material master batch prepared from third inorganic micro-nano particles and a third polymer substrate material according to a third weight proportion.
Preferably, the weight ratio of the inorganic micro-nano particles in the at least one third composite material master batch is 1% -80%, and the weight ratio of the inorganic micro-nano particles in the at least one third composite material master batch is greater than or equal to the weight ratio of the inorganic micro-nano particles in the second composite material master batch.
Preferably, the polymer base material includes one or a mixture of more than one of Polymethylmethacrylate (PMMA), fluororesin-modified polymethylmethacrylate (F-PMMA), Polyethylene (PE), polypropylene (PP), Polyamide (PA), polyethylene terephthalate (PET), polyvinylidene fluoride (PVDF), polyvinyl chloride (PVC), Polystyrene (PS), polyester and sodium sulfoisophthalate copolymer, acrylate copolymer, polyethylene glycol (PEG), polytrimethylene terephthalate (PTT), polyvinylidene chloride resin (PVDC), vinyl acetate resin, polyvinyl alcohol (PVA), and polyvinyl acetal.
Preferably, the inorganic micro-nano particles comprise titanium dioxide (TiO)2) Silicon dioxide (SiO)2) Zinc oxide (ZnO), silicon carbide (SiC), silicon nitride (Si)3N4) Zinc sulfide (ZnS), aluminum oxide (Al)2O3) Iron oxide (Fe)2O3) Boron Nitride (BN), magnesium oxide (MgO), barium sulfate (BaSO)4) Barium carbonate (BaCO)3) And aluminum silicate (Al)2SiO5) One or a mixture of more than one of them.
Preferably, the particle size range of the inorganic micro-nano particles is 0.03-250 μm.
Preferably, the monofilament fineness of the radiation refrigeration fiber ranges from 1D to 50D, and the fiber diameter ranges from 0.1mm to 1.5 mm.
Preferably, the radiation refrigeration fiber comprises at least one of a single structure, a sheath-core structure, a radial gradient concentration structure, a herringbone structure, a shaped convex structure, a segmented pie structure, a parallel structure, a rotational symmetric orientation structure, and an island-in-sea structure.
Preferably, the composite extrusion temperature is 100-600 ℃, and the winding speed is 10-6000 m/min.
The preparation method of the radiation refrigeration fiber fabric specifically comprises the step of preparing the radiation refrigeration fiber fabric through knitting and/or weaving.
Preferably, the radiation-cooled fabric produced by knitting and/or weaving, in particular comprises
The radiation refrigeration fiber is used as one of the warp and the weft, and other fibers are used as the other of the warp and the weft for weaving;
or the radiation refrigeration fibers are woven as warp yarns and weft yarns.
By the technical scheme, the technical scheme provided by the invention at least has the following advantages: according to the invention, high-concentration inorganic micro-nano particles are introduced into polymer fibers by using a melt composite spinning method, and the size of the micro-nano particles and the internal composite structure of the fibers are accurately regulated, so that the fibers have excellent daytime radiation refrigeration performance, high mechanical strength and high weaving performance, and the radiation refrigeration fabric suitable for cooling the surface of human skin is obtained, and has the advantages of large-scale batch preparation, low cost and high production efficiency.
According to the preparation method, the high-concentration inorganic micro-nano particles are introduced for doping, the particle size is accurately regulated and controlled, the radiation refrigeration performance is improved to the maximum extent, and the fiber and the fabric with excellent day and night radiation refrigeration performance are prepared.
The preparation method can be used for designing the internal composite structure of the fiber, so that the fiber has excellent radiation refrigeration performance, good mechanical property, elastic stability and high comfort.
Drawings
FIG. 1 is a schematic cross-sectional view of a radiation-cooled fiber prepared according to examples 1 and 2 of the present invention.
FIG. 2 is a schematic cross-sectional view of a radiation-cooled fiber prepared according to example 3 of the present invention.
FIG. 3 is a schematic cross-sectional view of a radiation-cooled fiber prepared according to example 4 of the present invention.
FIG. 4 is a schematic cross-sectional view of a radiation-cooled fiber prepared according to example 5 of the present invention.
FIG. 5 is a schematic cross-sectional view of a radiation-cooled fiber prepared according to example 6 of the present invention.
FIG. 6 is a schematic cross-sectional view of a radiation-cooled fiber prepared according to example 7 of the present invention.
FIG. 7 is a schematic cross-sectional view of a radiation-cooled fiber prepared according to example 8 of the present invention.
Fig. 8 is a schematic view of an apparatus for manufacturing a composite masterbatch according to an embodiment of the present invention.
FIG. 9 is a schematic view of an apparatus for melt spinning according to an embodiment of the present invention.
Fig. 10 is a schematic representation of a prepared radiation-cooled fiber of an embodiment of the present invention woven into a fabric.
The device comprises a feed port 1, a screw extruder 2, a melt extrusion port 3, a casting belt cooling device 4, a casting belt traction disc 5, a casting belt 6, a granulator 7, a master batch outlet 8, a composite master batch hopper 9, a spinning machine feed port 10, a screw extruder 11, a metering pump 12, a composite spinning assembly 13, radiation refrigeration fibers 14, an oil tanker 15, a yarn guide disc 16, a winding drum 17, a first component 20, a second component 30 and a third component 40.
Detailed Description
Exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention can be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The prepared radiation refrigeration fiber fabric comprises a polymer substrate and inorganic micro-nano particles, the inorganic micro-nano particles are dispersed in the polymer substrate, and the radiation refrigeration fiber and the fabric thereof are prepared by a melt spinning method, and the method specifically comprises the following steps:
101: preparing the radiation refrigeration composite material master batch, namely uniformly mixing the inorganic micro-nano particles and the polymer substrate material according to a preset weight ratio to prepare the composite material master batch.
102: and (3) performing melt spinning to obtain radiation refrigeration fibers, performing extrusion molding on the composite material master batch obtained in the step (101) in a spinning assembly, and winding to obtain the radiation refrigeration fibers.
103: and (3) preparing the radiation refrigerating fabric, namely weaving the radiation refrigerating fibers obtained in the step (102) through a knitting and/or weaving process to form the radiation refrigerating fabric.
Preferably, the step 101 specifically includes uniformly mixing the first inorganic micro-nano particles and the first polymer base material according to a predetermined first weight ratio to obtain first composite material master batches, and uniformly mixing the second inorganic micro-nano particles and the second polymer base material according to a predetermined second weight ratio to obtain second composite material master batches;
the weight ratio of the inorganic micro-nano particles in the first composite material master batch is 1-80 wt.%, the weight ratio of the inorganic micro-nano particles in the second composite material master batch is 0-20 wt.%, and the weight ratio of the inorganic micro-nano particles in the first composite material master batch is more than or equal to that of the inorganic micro-nano particles in the second composite material master batch.
And the step 102 comprises the steps of taking the first composite material master batch obtained in the step 101 as a first component, taking the second composite material master batch as a second component, carrying out composite extrusion molding in a spinning assembly, and winding to obtain the radiation refrigeration fiber.
The first composite material master batch and the second composite material master batch of the radiation refrigeration fiber are both prepared by mixing inorganic micro-nano particles with polymer substrates in different weight proportions in a high concentration mode, the first polymer substrate material in the first composite material master batch and the second polymer substrate material in the second composite material master batch can be the same or different, and the first weight proportion is more than or equal to the second weight proportion, so that the first component in the radiation refrigeration fiber can be a highly doped composite material, and the second component can be low-doped or zero-doped, so that the whole radiation refrigeration fiber can ensure certain toughness and can be easily woven into a fabric. Similarly, the first inorganic micro-nano particles in the first composite material master batch and the second inorganic micro-nano particles in the second composite material master batch can be the same or different, preferably, the first inorganic micro-nano particles and the second inorganic micro-nano particles are the same.
In addition, as another embodiment of the present invention, the radiation refrigeration fiber may further include at least one third component, where the third component corresponds to a third composite material mother particle prepared from a third inorganic micro-nano particle and a third polymer base material according to a third weight ratio, the weight ratio of the inorganic micro-nano particles in the at least one third composite material mother particle is 1 to 80 wt.%, and the weight ratio of the inorganic micro-nano particles in the at least one third composite material mother particle is greater than or equal to the weight ratio of the inorganic micro-nano particles in the second composite material mother particle. When the number of the at least one third component is at least two, at least one parameter of the at least two third components is different from at least one parameter of the inorganic micro-nano particles, the particle size of the inorganic micro-nano particles, the mass ratio of the inorganic micro-nano particles and the polymer substrate material.
Preferably, in step 103, the radiation refrigeration fibers obtained in step 102 may be used to weave a fabric alone, or the radiation refrigeration fibers may be used as one of the weft and the warp, and the other fibers are used as the other of the warp and the weft, which are mixed to form the radiation refrigeration fabric. The other fibers can be fibers of other single fabrics or blended fabrics such as terylene, cotton and the like.
The polymer base material is thermoplastic resin, preferably, one or a mixture of more than one of polymethyl methacrylate (PMMA), fluororesin-modified polymethyl methacrylate (F-PMMA), Polyethylene (PE), polypropylene (PP), Polyamide (PA), polyethylene terephthalate (PET), polyvinylidene fluoride (PVDF), polyvinyl chloride (PVC), Polystyrene (PS), polyester/sodium isophthalate copolymer, acrylate copolymer, polyethylene glycol (PEG), polytrimethylene terephthalate (PTT), polyvinylidene chloride resin (PVDC), vinyl acetate resin, polyvinyl alcohol (PVA), polyvinyl acetal, and the like.
Preferably, in the fluororesin-modified polymethyl methacrylate (F-PMMA), the mass ratio of the fluororesin to PMMA is in the range of 1:100 to 10: 1.
Preferably, the inorganic micro-nano particles comprise titanium dioxide (TiO)2) Silicon dioxide (SiO)2) Zinc oxide (ZnO), silicon carbide (SiC), silicon nitride (Si)3N4) Zinc sulfide (ZnS), aluminum oxide (Al)2O3) Iron oxide (Fe)2O3) Boron Nitride (BN), magnesium oxide (MgO), barium sulfate (BaSO)4) Barium carbonate (BaCO)3) And aluminum silicate (Al)2SiO5) And the like, or a mixture of more than one thereof. Preferably, the inorganic micro-nano particles are TiO2。
The particle size range of the inorganic micro-nano particles is 0.03-250 μm, preferably, the particle size of the micro-nano particles is 0.4-1.2 μm, and further preferably, 0.6 μm.
The radiation refrigeration fiber has the filament number range of 1D-50D and the fiber diameter range of 0.1mm-1.5 mm.
When the materials of the second and third components are added to the first component, the radiation refrigeration fiber with a composite structure can be obtained, and for example, the radiation refrigeration fiber can be at least one of a sheath-core structure, a radial gradient concentration structure, a herringbone structure, a special-shaped convex structure, a orange-lobe structure, a parallel structure, a rotational symmetric orientation structure, an island-in-sea structure and other composite structures. While when the second component material is the same as the polymeric base material in the first component, the melt-extruded radiation-cooled fiber remains a unitary structure, except that the shape can be controlled as desired.
Extruding and molding the composite master batch in a spinning assembly, and winding to obtain the radiation refrigeration fiber, wherein the first component and the second component are extruded and molded in the spinning assembly, and the temperature of the composite extrusion molding is 100-600 ℃, and the preferred temperature range is 150-350 ℃; the winding speed is 10m/min-6000m/min, preferably 200m/min-500m/min, more preferably 300 m/min.
The process for preparing the composite material master batch specifically comprises the steps of carrying out melt extrusion on a mixed material of the inorganic micro-nano particles and the polymer substrate material, carrying out water bath granulation, and then obtaining the radiation refrigeration composite material master batch, wherein the temperature range of the melt-extruded master batch is preferably 100-600 ℃, and more preferably 150-350 ℃.
Example 1:
in this example 1, the radiation refrigeration fiber only includes the first component, that is, the radiation refrigeration fiber with a single structure, and the cross section of the radiation refrigeration fiber is shown in fig. 1, a polymer substrate of the radiation refrigeration fiber is Polyethylene (PE), and the doped inorganic micro-nano particles are TiO2，TiO2The particle size of the particles was 600nm, and the weight ratio was 50 wt.%.
The method comprises the following specific steps:
101, preparing a radiation refrigeration composite material master batch;
using the apparatus shown in fig. 8, 1200g of Polyethylene (PE) particles were pulverized to powder and added to 1200g of TiO dried in a vacuum oven at 100 ℃ for 24 hours2The particles are mixed evenly. The mixed material was extruded through a twin screw extruder at 260 ℃ under 4MPa to form a melt cast strip. Solidifying the cast strip through a normal temperature water bath, guiding the cast strip to pass through a guide wheel to a slicer, and cutting the solidified melt cast strip into PE and TiO2、TiO2The weight ratio of the composite material master batch is 50 percent.
102, preparing radiation refrigerating fibers by melt spinning;
using the apparatus shown in FIG. 9, PE and TiO were mixed2And drying the composite master batch in a vacuum oven at 75 ℃ for 24 h. Will be driedFilling the finished composite material master batch into a hopper of a melt spinning machine, and adjusting the temperature of each area of the melt spinning machine, such as: the temperature of each zone of the screw is divided into four zones, namely 235 ℃, 260 ℃, 275 ℃ and 275 ℃, the temperature of the metering pump is 275 ℃, and the temperature of the spinning assembly is 280 ℃. Carrying out melt composite spinning to prepare fibers under the conditions that the rotating speed of a screw is 20Hz and the pressure of a stable screw is 5.6MPa, and winding at a winding speed of 300m/min to obtain the radiation refrigeration fibers uniformly doped with 50 wt.% of titanium dioxide particles.
(3) Preparing a radiation refrigerating fabric;
the obtained radiation refrigeration fibers are used as weft yarns, and the radiation refrigeration fibers with proper length and number are taken to pass through heddle eyes and reed teeth of a shuttle loom and are arranged in a harness frame in order to be used as warp yarns, so that the fibers are prevented from being worn by an excessively strong friction effect, and the warp yarns of the cloth roller are adjusted to ensure uniform tension and proper tightness; according to the change rule of warp and weft interweaving, an upper layer of warp and a lower layer of warp are driven in sequence by utilizing a shedding mechanism to form a shed channel; and winding fibers on a shuttle to serve as weft yarns, weaving the shuttle through a shed channel in a reciprocating and alternating manner, adjusting the arrangement density of the weft yarns by matching with other mechanisms on a weaving machine, and winding and leading off the fabric on a cloth roller, thereby obtaining the radiation refrigeration fabric uniformly doped with 50 wt.% of titanium dioxide particles. As shown in fig. 10.
Example 2:
as shown in fig. 1, this embodiment is also a radiation refrigeration fiber with a single structure, a polymer substrate of the radiation refrigeration fiber is polypropylene (PP) which is a polymer material, and the doped inorganic micro-nano particles are TiO2，TiO2The particles had a particle size of 600nm and a weight proportion of 20 wt.%. The radiation refrigeration fiber comprises two components during manufacturing, wherein the polymer substrate materials and the inorganic micro-nano particles of the first component and the second component are the same, and the weight ratio is also the same.
The specific manufacturing method comprises the following steps:
101, preparing a radiation refrigeration composite material master batch:
pulverizing 1200g of polypropylene (PP) particles to powder, adding 300g of TiO dried in a vacuum oven at 100 ℃ for 24h2Particle mixingAnd (4) uniformity. The mixed material was extruded through a twin screw extruder at 260 ℃ under 4MPa to form a melt cast strip. Solidifying the casting belt through water bath, guiding the casting belt to pass through a guide wheel to a granulator, and cutting the solidified melt casting belt into PP and TiO2、TiO 220% by weight of the composite master batch.
102, preparing radiation refrigeration fibers by melt composite spinning:
mixing PP and TiO2The master batch of the composite material is dried for 24 hours in a vacuum oven at the temperature of 75 ℃. The dried PP @ TiO is added2(20 wt.%) of composite master batch, which is used as a first component and a second component, respectively, filling the first component and the second component into two hoppers of a melt spinning machine, adjusting the temperature and the screw rotation speed of each area of the melt spinning machine, stabilizing the screw pressure, preparing the single-structure radiation refrigerating fiber by melt composite spinning, and collecting and doffing the single-structure radiation refrigerating fiber at a winding speed of 300m/min, thereby obtaining the single-structure radiation refrigerating fiber uniformly doped with 20 wt.% titanium dioxide particles.
103, preparation of radiation refrigerating fabric:
the obtained radiation refrigeration fibers are used as weft yarns, the radiation refrigeration fibers with proper length and number are taken to pass through heddle eyes and reed teeth of a shuttle loom and are arranged in a harness frame in order to be used as warp yarns, and in order to avoid the fibers from being worn by an over-strong friction effect, the warp yarns of a cloth roller are adjusted to ensure uniform tension and proper tightness; according to the change rule of warp and weft interweaving, an upper layer of warp and a lower layer of warp are driven in sequence by utilizing a shedding mechanism to form a shed channel; and winding fibers on a shuttle to serve as weft yarns, weaving the shuttle through a shed channel in a reciprocating and alternating manner, adjusting the arrangement density of the weft yarns by matching with other mechanisms on a weaving machine, and winding and leading off the fabric on a cloth roller, thereby obtaining the radiation refrigeration fabric uniformly doped with 20 wt.% of titanium dioxide particles.
Example 3:
as shown in fig. 2, the radiation refrigeration fiber prepared in this embodiment has a core-skin structure, that is, includes two components, a first component 20 and a second component 30, a polymer base material of the first component 20 is a composite material (F-PMMA) of fluororesin and polymethyl methacrylate, and doped inorganic micro-nano particles are TiO2And is micro-nano particleGranular TiO2Has a particle size of 600nm and a first weight proportion of 60 wt.%. The polymer substrate material in the second component 30 is F-PMMA, and the micro-nano particles are zero-doped.
The preparation method comprises the following steps:
101, preparation of radiation refrigeration composite material master batch
Pulverizing 10g of fluororesin particles and 1000g of PMMA particles to powder, adding 1515g of TiO2The particles are mixed uniformly, the TiO2The granules are dried in a vacuum oven for 24 hours at 100 ℃. The mixed material was extruded through a twin screw extruder at 260 ℃ under 4MPa to form a melt cast strip. Solidifying the cast strip through a normal temperature water bath, guiding the cast strip to pass through a guide wheel to a slicer, and slicing the solidified melt cast strip to obtain F-PMMA (1:100) and TiO2(60 wt.%) of the composite masterbatch, i.e. the first composite masterbatch.
And similarly, mixing the fluororesin particles and the PMMA particles, and crushing into powder to prepare F-PMMA composite material master batch, namely the second composite material master batch.
102, preparing radiation refrigeration fibers by melt composite spinning:
mixing F-PMMA and TiO2(60 wt.%) of the composite masterbatch was dried in a vacuum oven at 75 ℃ for 24 h. Filling the dried composite material master batches and the F-PMMA composite material master batches into a hopper of a melt spinning machine respectively, adjusting the temperature and the screw rotating speed of each area of the melt spinning machine, stabilizing the screw pressure, preparing the skin-core structure radiation refrigerating fiber by melt composite spinning, and winding and doffing at the winding speed of 300m/min to obtain the skin-core structure radiation refrigerating fiber with the core layer uniformly doped with 60 wt.% of titanium dioxide particles. The first component serves as a core layer and the second component serves as a cladding layer.
103, the procedure for preparing the radiation refrigerating fabric was the same as in example 1, thereby obtaining a skin-core structure radiation refrigerating fabric in which the core layer of the fiber was uniformly doped with 60 wt.% titanium dioxide particles.
Example 4
As shown in fig. 3, the cross section of the radiation refrigeration fiber is in a form that the concentration, namely the weight concentration of the micro-nano particles is reduced along the radial direction. The fiber comprises a first groupA component 20, a second component 30, and a third component 40. The polymer substrate materials of the first component, the second component and the third component are both composite materials (F-PMMA) of fluororesin and polymethyl methacrylate, and the doped inorganic micro-nano particles are TiO micro-nano particles2The particle size is 600 nm. The weight ratio of the micro-nano particles in the first component is 80%. The weight proportion of the micro-nano particles in the third component is 60%, and the weight proportion of the micro-nano particles in the second component is 0 without doping. The first component 20, the third component 40 and the second component 30 are sequentially arranged from inside to outside, so that the weight ratio of the micro-nano particles is reduced along the radial direction.
The preparation method of the radiation refrigeration fiber in the embodiment comprises the following steps:
101, preparing a radiation refrigeration composite material master batch;
pulverizing 10g of fluororesin particles and 1000g of PMMA particles into powder, adding 4040g of TiO2The particles are mixed uniformly, the TiO2Drying in a vacuum oven at 100 ℃ for 24 h. Extruding the mixed material through a double-screw extruder at 260 ℃ and 4MPa to obtain a melt casting belt, solidifying the casting belt through a normal-temperature water bath, guiding the casting belt to pass through a guide wheel to a slicer, and slicing the solidified melt casting belt to obtain F-PMMA (1:100) and TiO2(80 wt.%) of the composite masterbatch, i.e. the first composite masterbatch.
And in the same way, F-PMMA (1:100) and TiO are prepared2(60 wt.%) of the master batch of the composite material, namely the master batch of the third composite material, and preparing the master batch of the F-PMMA composite material, namely the master batch of the second composite material in the same way.
102, preparing radiation refrigerating fibers by melt composite spinning;
and (3) drying the three composite material master batches prepared in the step (101) in a vacuum oven at the temperature of 75 ℃ for 24 hours. F-PMMA and TiO after the drying is finished2(80 wt.%) composite masterbatch, F-PMMA and TiO2(60 wt.%) the composite master batch and the F-PMMA composite master batch are respectively filled in a hopper of a melt spinning machine, the temperature and the screw rotating speed of each area of the melt spinning machine are adjusted, the screw pressure is stabilized, the radial gradient concentration structure radiation refrigeration fiber is prepared by melt composite spinning, and the radial gradient concentration structure radiation refrigeration fiber is wound at the winding speed of 300m/minAnd (3) spinning, thereby obtaining the radial gradient concentration structure radiation refrigeration fiber, wherein the innermost core layer is uniformly doped with 80 wt.% titanium dioxide particles, and the middle layer is uniformly doped with 60 wt.% titanium dioxide particles.
103, preparing a radiation refrigerating fabric;
taking the obtained radiation refrigeration fibers as weft yarns, taking other fibers with proper length and number to pass through heddle eyes and reed teeth of a shuttle loom, and neatly arranging the fibers in a heald frame as warp yarns, so that the fibers are prevented from being worn by an excessively strong friction effect, and the warp yarns of the cloth roller are adjusted to ensure uniform tension and proper tightness; according to the change rule of warp and weft interweaving, an upper layer of warp and a lower layer of warp are driven in sequence by utilizing a shedding mechanism to form a shed channel; and winding fibers on the shuttle to be used as weft yarns, weaving the shuttle through a shed channel in a reciprocating and alternating manner, adjusting the arrangement density of the weft yarns by matching with other mechanisms on a weaving machine, and winding and leading off the fabric on a cloth roller, thereby obtaining the radiation refrigeration fabric doped with titanium dioxide particles. The other fibers can be fibers of other fabrics such as terylene, cotton and the like, and can be selected according to the requirement.
The mechanical properties of the composite radiation refrigeration fibers in examples 1, 2, 3 and 4 were compared, and are shown in table 1. Under the same external conditions, the breaking strength of the sheath-core structural fiber of example 3 and the radial gradient concentration structural composite fiber of example 4 is much higher than that of the single structural composite fibers of examples 1 and 2. This is because the mechanical properties of the fiber are greatly enhanced by the sheath of the composite fiber prepared by the melt composite spinning method. Due to the influence of doping concentration, the fabrics of single structures prepared in examples 1 and 2 have lower reflectivity of solar radiation compared with the radiation refrigeration fibers of the sheath-core structure in example 3 and the radial gradient concentration structure in example 4. The method shows that the concentration of the doped micro-nano particles and the internal structure of the fiber are adjusted by a melt composite spinning method, so that the radiation performance is ensured, and the mechanical strength is good, and the method is suitable for manufacturing the fabric for cooling the surface of the human body.
TABLE 1
Examples Fiber structure Highest micro-nano particle doping concentration in fiber
Example 1 Unitary structure 20wt.％
Example 2 Unitary structure 50wt.％
Example 3 Skin-core structure 60wt.％
Example 4 Radial gradient concentration structure 80wt.％
Example 5:
the fiber in this embodiment is a radiation refrigerating fiber with a cross section of a heterosexual structure, as shown in fig. 4, the radiation refrigerating fiber comprises a first component 20 and a second component 30, the first component 20 is located at the center and is a core layer, the second component 30 is located at the outer side and is a cladding layer, and the cladding layer comprises protrusions which are uniformly distributed along the circumferential direction at the outer side of the core layer. The polymer substrate material in the first component 20 is Polyamide (PA), wherein the doped inorganic micro-nano particles are TiO2Average particle size of about 600nm, TiO2The doping concentration was 50 wt.%. The polymer base material of the second component 30 is a composite material (F-PMMA) of fluororesin and polymethyl methacrylate) And the mass ratio of the inorganic micro-nano particles is 0, namely zero doping.
The preparation method of the radiation refrigeration fiber and the fabric thereof comprises the following steps:
101, preparing a radiation refrigeration composite material master batch:
pulverizing 1200g of Polyamide (PA) particles to powder, adding 1200g of TiO dried in a vacuum oven at 100 deg.C for 24h2The particles are mixed evenly. The mixed material was extruded through a twin screw extruder at 260 ℃ under 4MPa to form a melt cast strip. Solidifying the cast strip through a normal temperature water bath, guiding the cast strip to pass through a guide wheel to a slicer, and cutting the solidified melt cast strip into PA and TiO2(50 wt.%) of the composite masterbatch, i.e. the first composite masterbatch. 1000g of fluororesin particles and 100g of PMMA particles were pulverized into a powder, and the mixed material was extruded from a melt cast ribbon through a twin-screw extruder at 260 ℃ under a pressure of 4 MPa. And (3) solidifying the casting belt through a normal-temperature water bath, guiding the casting belt to pass through a guide wheel to a slicing machine, and slicing the solidified melt casting belt to obtain F-PMMA (10:1) composite material master batches, namely second composite material master batches.
102, preparing radiation refrigeration fibers by melt composite spinning:
mixing PA and TiO2(50 wt.%) and F-PMMA composite masterbatch were dried in a vacuum oven at 75 ℃ for 24 h. Drying the PA and TiO2(50 wt.%) composite master batch and F-PMMA composite master batch are respectively filled in a hopper of a melt spinning machine, the temperature and the screw rotating speed of each area of the melt spinning machine are adjusted, the screw pressure is stabilized, the special-shaped structure radiation refrigeration fiber is prepared by melt composite spinning, and the special-shaped structure radiation refrigeration fiber is obtained by winding at the winding speed of 300m/min, so that the special-shaped structure radiation refrigeration fiber with the core layer uniformly doped with 50 wt.% titanium dioxide particles and the outer layer protruding in an arc shape is obtained.
(3) The preparation steps of the radiation refrigeration fabric are the same as those of the example 1, so that the radiation refrigeration fabric with the special-shaped structure, the core layer of which is uniformly doped with 50 wt.% of titanium dioxide particles and the outer layer of which is arc-shaped and convex, is obtained.
Compared with the composite material radiation refrigeration fiber in the embodiment 1 and the embodiment 5, the radiation refrigeration fiber in the embodiment 5 is externally provided with a plurality of convex special-shaped structures, so that the surface of the fiber is provided with grooves, and compared with the radiation refrigeration fiber in the circular structure in the embodiment 1, the radiation refrigeration fiber in the embodiment has larger surface area, thereby being capable of enhancing the moisture absorption and sweat releasing performance of the fiber. And the modification of the fluororesin makes the fiber more flexible. Therefore, the internal structure of the fiber is regulated and controlled through melt composite spinning, and the comfort is enhanced while the radiation refrigeration performance of the fiber is maintained.
Example 6:
as shown in fig. 5, the radiation refrigerating fiber prepared in this example has a circular cross section, includes a first component 20 and a second component 30, and the first component 20 and the second component 30 are respectively shaped as semi-circles in the circle. The polymer base material in the first component 20 is polytrimethylene terephthalate (PTT), and the inorganic micro-nano particles in the first component 20 are TiO250 wt.% in mass; the polymer base material in the second component 30 is polyethylene terephthalate (PET), and the mass ratio of the inorganic micro-nano particles in the second component 30 is 0, that is, zero doping.
The preparation method of the radiation refrigeration fiber comprises the following steps:
101, preparing a radiation refrigeration composite material master batch:
pulverizing 1200g polytrimethylene terephthalate (PTT) particles to powder, adding 1200g TiO dried in a vacuum oven at 120 deg.C for 24h2The particles are mixed evenly. The mixed material was extruded through a twin screw extruder at 290 ℃ under 6MPa to form a melt cast strip. Solidifying the cast strip through a normal temperature water bath, guiding the cast strip to pass through a guide wheel to a slicer, and cutting the solidified melt cast strip into PTT and TiO2(50 wt.%) of the composite masterbatch.
Preparing the PET master batch in the same way.
102, preparing radiation refrigeration fibers by melt composite spinning:
mixing PTT and TiO2(50 wt.%) the composite masterbatch was dried in a vacuum oven at 120 ℃ for 24 h. PTT and TiO after drying is finished2(50 wt.%) composite master batch and PET master batch are respectively filled in hopper of melt spinning machine, and the temp. and screw rotation speed of each region of melt spinning machine are regulated to stabilizeScrew pressure, melt composite spinning to prepare radiation refrigeration fiber with a parallel structure, and winding and doffing at a winding speed of 300m/min to obtain radiation refrigeration fiber with a parallel structure, wherein half of the radiation refrigeration fiber is polyethylene terephthalate (PET) and half of the radiation refrigeration fiber is polytrimethylene terephthalate (PTT) uniformly doped with 50 wt.% titanium dioxide particles.
103, the radiation refrigerating fabric was prepared in the same manner as in example 1, thereby obtaining a side-by-side structure radiation refrigerating fabric of polyethylene terephthalate (PET) in half and polytrimethylene terephthalate (PTT) in half doped with 50 wt.% titanium dioxide particles.
The composite radiation refrigeration fibers of examples 2 and 6 were taken for comparison. The radiation refrigeration prepared in example 6 is a side-by-side structure fiber of polyethylene terephthalate (PET) in half and polytrimethylene terephthalate (PTT) in half uniformly doped with 50 wt.% titanium dioxide particles, and due to different orientations and crystalline structures of the two components, there is a difference in thermal shrinkage rate between the two, and after heating, the two components have different shrinkage stresses to generate a differential shrinkage effect, which causes the whole fiber to spontaneously twist, and thus the fiber has different degrees of elasticity and elasticity. Compared with the circular-structure radiation refrigeration fiber in the embodiment 2, the parallel-structure fiber and the fabric thereof have excellent radiation refrigeration performance and good crimp stability. Therefore, the internal structure of the fiber is regulated and controlled through the melt composite spinning, and the comfort is greatly enhanced while the radiation refrigeration performance of the fiber is maintained.
Example 7:
as shown in fig. 6, the radiation refrigeration fiber with a segmented pie cross section comprises two components, wherein a polymer base material of a first component 20 is nylon 6(PA6), and doped inorganic micro-nano particles are TiO2Average particle size about 600nm, and doping concentration in PA6 of 50 wt.%. The polymer base material of the second component 30 is polytrimethylene terephthalate (PTT), and the inorganic micro-nano particles are zero-doped.
The preparation method of the radiation refrigeration fiber comprises the following steps:
101, preparing a radiation refrigeration composite material master batch:
1200g of nylon 6(PA6) granules were ground to a powder and 1200g of TiO was added2The particles are mixed uniformly, the TiO2The granules are dried in a vacuum oven for 24 hours at 120 ℃. The mixed material was extruded through a twin screw extruder at 270 ℃ under a pressure of 4MPa to form a melt cast strip. Solidifying the cast strip through a normal temperature water bath, guiding the cast strip through a guide wheel to a slicer, and cutting the solidified melt cast strip into PA6 and TiO 62(50 wt.%) of the composite masterbatch.
(2) Preparing radiation refrigeration fiber by melt composite spinning:
mixing PA6 with TiO2(50 wt.%) the composite masterbatch was dried in a vacuum oven at 120 ℃ for 24 h. Drying the PA6 and TiO2(50 wt.%) of the composite master batch and the PTT master batch are respectively filled in a hopper of a melt spinning machine, the temperature and the screw rotating speed of each zone of the melt spinning machine are adjusted, the screw pressure is stabilized, the orange-petal-structure radiation refrigeration fiber is prepared by melt composite spinning, and the orange-petal-structure radiation refrigeration fiber doped with 50 wt.% of titanium dioxide particles is obtained by winding at a winding speed of 300m/min and doffing.
(3) The preparation steps of the radiation refrigeration fabric are the same as those of the example 1, so that the radiation refrigeration fabric with the orange-peel structure doped with titanium dioxide particles is obtained.
Example 8:
as shown in fig. 7, the cross section of the radiation refrigeration fiber is in a sea island shape, wherein the polymer base material of the first component 20 is polyethylene terephthalate (PET), and the inorganic micro-nano particles doped therein are TiO2Average particle size 600nm, doping concentration in PET 50 wt.%. The polymer substrate material of the second component 30 is Polystyrene (PS), and the inorganic micro-nano particles are zero-doped.
The preparation method of the fiber comprises
101, preparing a radiation refrigeration composite material master batch:
1200g of polyethylene terephthalate (PET) granules were pulverized into powder, and 1200g of TiO was added2The particles are mixed uniformly, the TiO2The granules are dried in a vacuum oven for 24 hours at 120 ℃. Extruding the mixed material by a double-screw extruder at 280 ℃ and 4MPaAnd (4) discharging the melt cast strip. Solidifying the cast strip through a normal temperature water bath, guiding the cast strip to pass through a guide wheel to a slicer, and cutting the solidified melt cast strip into PET and TiO2(50 wt.%) of the composite masterbatch.
(2) Preparing radiation refrigeration fiber by melt composite spinning:
mixing PET and TiO2(50 wt.%) the composite masterbatch was dried in a vacuum oven at 120 ℃ for 24 h. Drying the PET and TiO2(50 wt.%) of the composite masterbatch and Polystyrene (PS) masterbatch are respectively filled in a hopper of a melt spinning machine, the temperature and the screw rotating speed of each region of the melt spinning machine are adjusted, the screw pressure is stabilized, the sea-island structure radiation refrigeration fiber is prepared by melt composite spinning, and the fiber is wound and doffed at a winding speed of 300m/min, so that the sea-island structure radiation refrigeration fiber doped with 50 wt.% titanium dioxide particles is obtained.
(3) The procedure for preparing the radiation refrigerating fabric was the same as in example 1, thereby obtaining an island structure radiation refrigerating fabric doped with 50 wt.% titanium dioxide particles.
The composite radiation refrigeration fibers of examples 2, 7 and 8 were taken for comparison. The radiation refrigeration fibers prepared in the examples 7 and 8 have good refrigeration performance and mechanical strength. Compared with the single-structure radiation refrigeration fiber prepared in the embodiment 2, the fabric prepared from the superfine fiber has excellent radiation refrigeration performance and higher softness and comfort. And a porous hollow fiber having elasticity can be obtained by removing the island component of the sea-island structure fiber prepared in example 8. Therefore, the internal structure of the fiber is regulated and controlled through the melt composite spinning, the fabric gloss is soft while the radiation refrigeration performance is maintained, the wearing comfort level is greatly improved, and the high-grade spinning fabric suitable for cooling the skin of a human body can be woven.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above are merely examples of the present application and are not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.

Claims (14)

1. A method of making a radiation-cooled fiber, comprising:
mixing the inorganic micro-nano particles and the polymer substrate material according to a preset weight ratio to prepare a composite material master batch;
and carrying out composite extrusion molding on the composite master batch in a spinning assembly, and winding to obtain the radiation refrigeration fiber.
2. A method of making a radiation-curable fiber of claim 1, wherein: the inorganic micro-nano particles and the polymer substrate material are mixed according to a preset weight proportion to prepare the composite material master batch, which comprises,
uniformly mixing first inorganic micro-nano particles and a first polymer base material according to a preset first weight ratio to prepare a first composite material master batch, and uniformly mixing second inorganic micro-nano particles and a second polymer base material according to a preset second weight ratio to prepare a second composite material master batch;
and extruding and molding the composite material master batch in a spinning assembly, and winding to obtain the radiation refrigeration fiber.
3. A method of making a radiation-curable fiber of claim 2, wherein: the weight proportion of the inorganic micro-nano particles in the first composite material master batch is 1-80%, the weight proportion of the inorganic micro-nano particles in the second composite material master batch is 0-20%, and the weight proportion of the inorganic micro-nano particles in the first composite material master batch is more than or equal to that of the inorganic micro-nano particles in the second composite material master batch.
4. A method of making a radiation-curable fiber of claim 3, wherein: the first polymer substrate material and the second polymer substrate material may be the same or different; the first inorganic micro-nano particles and the second inorganic micro-nano particles can be the same or different.
5. A method of making a radiation-curable fiber of claim 2, wherein: the radiation refrigeration fiber is prepared by carrying out composite extrusion molding on the at least one third component, the first component and the second component in a spinning assembly, and winding;
the at least one third component is at least one third composite material master batch prepared from third inorganic micro-nano particles and a third polymer substrate material according to a third weight proportion.
6. A method of making a radiation-curable fiber of claim 5, wherein: the weight proportion of the inorganic micro-nano particles in the at least one third composite material master batch is 1% -80%, and the weight proportion of the inorganic micro-nano particles in the at least one third composite material master batch is more than or equal to the weight proportion of the inorganic micro-nano particles in the second composite material master batch.
7. A method of making a radiation refrigerating fiber as claimed in any one of claims 1 to 6, wherein: the polymer base material comprises one or a mixture of more than one of polymethyl methacrylate (PMMA), fluororesin modified polymethyl methacrylate (F-PMMA), Polyethylene (PE), polypropylene (PP), Polyamide (PA), polyethylene terephthalate (PET), polyvinylidene fluoride (PVDF), polyvinyl chloride (PVC), Polystyrene (PS), polyester and sodium isophthalate copolymer, acrylate copolymer, polyethylene glycol (PEG), polytrimethylene terephthalate (PTT), polyvinylidene chloride resin (PVDC), vinyl acetate resin, polyvinyl alcohol (PVA) and polyvinyl acetal.
8. A method of making a radiation refrigerating fiber as claimed in any one of claims 1 to 6, wherein: the inorganic micro-nano particles comprise titanium dioxide (TiO)2) Silicon dioxide (SiO)2) Zinc oxide (ZnO), silicon carbide (SiC), silicon nitride (Si)3N4) Zinc sulfide (ZnS), aluminum oxide (Al)2O3) Iron oxide (Fe)2O3) Boron Nitride (BN), magnesium oxide (MgO), barium sulfate (BaSO)4) Barium carbonate (BaCO)3) And aluminum silicate (Al)2SiO5) One or a mixture of more than one of them.
9. A method of making a radiation refrigerating fiber as claimed in any one of claims 1 to 6, wherein: the particle size range of the inorganic micro-nano particles is 0.03-250 mu m.
10. A method of making a radiation refrigerating fiber as claimed in any one of claims 1 to 6, wherein: the single filament number range of the radiation refrigeration fiber is 1D-50D, and the fiber diameter range is 0.1mm-1.5 mm.
11. A method of making a radiation refrigerating fiber as claimed in any one of claims 1 to 6, wherein: the radiation refrigeration fiber comprises at least one of a single structure, a sheath-core structure, a radial gradient concentration structure, a herringbone structure, a special-shaped convex structure, a orange lobe structure, a parallel structure, a rotational symmetric azimuth structure and an island-in-sea structure.
12. A method of making a radiation refrigerating fiber as claimed in any one of claims 1 to 6, wherein: the composite extrusion temperature is 100-600 ℃, and the winding speed is 10-6000 m/min.
13. A method for preparing a radiation refrigeration fiber fabric, which comprises the step of knitting and/or weaving the radiation refrigeration fiber obtained in the claims 1-12 to obtain the radiation refrigeration fiber fabric.
14. A method of making a radiation-cooled fibrous web of claim 13, wherein: the radiation refrigerating fabric is prepared by knitting and/or weaving, and specifically comprises
The radiation refrigeration fiber is used as one of the warp and the weft, and other fibers are used as the other of the warp and the weft for weaving;
or the radiation refrigeration fibers are woven as warp yarns and weft yarns.
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