CN115341302B - Preparation method of sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber - Google Patents
Preparation method of sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber Download PDFInfo
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to a preparation method of a skin-core type photo-thermal conversion-heat storage temperature regulation polyester fiber, which comprises the following steps: preparing photo-thermal conversion cellulose-based aerogel based on nano-cellulose and photo-thermal conversion zirconium carbide nano-material, and carbonizing to obtain a composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material; grinding and carrying out surface hydrophobic modification; extruding and granulating the polyester chip and the hydrophobic-composite photo-thermal conversion carbon aerogel powder to obtain photo-thermal conversion carbon aerogel functional master batch; preparing PEG-PET solid-solid phase change master batch; extruding the photo-thermal conversion carbon aerogel functional master batch and the PEG-PET solid-solid phase change master batch, and spinning to obtain the skin-core type photo-thermal conversion-heat storage temperature adjustment polyester fiber. Compared with the prior art, the skin-core type photo-thermal conversion-heat storage temperature regulation polyester fiber prepared by the invention is used as a photo-thermal material, and has the advantages of strong photo-absorption capacity, high photo-thermal conversion efficiency, good heat preservation performance, low cost and environmental protection.
Description
Technical Field
The invention relates to the field of functional fiber preparation, in particular to a preparation method of a sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber.
Background
The warm keeping and cold resisting clothing is a main function of winter clothing, the traditional warm keeping clothing mainly prevents heat loss of a body, and particularly in severe cold areas, people need to wear thicker clothing for keeping warm, so that comfort and activities of the body are very unfavorable, and the clothing capable of actively producing heat and being light, thin and warm is a great improvement of traditional textiles. Therefore, aiming at the development of green and the pursuit of people for wearing 'comfort, warmth retention and portability', the heat storage and temperature adjustment fiber with the light-heat conversion function is developed to become a new pet in the market.
The photo-thermal conversion and heat accumulation temperature regulation fiber is a functional fiber which can convert absorbed solar energy into heat energy, store the heat and achieve the energy accumulation and temperature control effect by regulating the microenvironment between the fabric and the human body. The single-function thermal fiber has the defects that the thermal effect is limited by factors such as environment, heating materials and the like due to the limitation of the material, and certain condition excitation is needed or the heating effect cannot be durable. Therefore, materials integrating light-heat conversion and energy storage are being developed in competition. Patent CN 102605614B discloses a preparation method of a bi-directional temperature-regulating fiber combining a photo-thermal material and a phase-change energy storage technology, the material can actively generate heat and store energy, and has better warmth retention property, but the fiber adopts the technologies of sizing, padding, coating and the like, belongs to the post-finishing technology of the fiber, and has the defects that a heating material is easy to fall off, is not resistant to friction, water washing and the like. Patent CN 110528097B discloses a photo-thermal conversion-heat storage temperature regulation cellulose fiber and a preparation method thereof, wherein the fiber has better photo-thermal conversion and energy storage performance, but the heat resistance of functional materials is the problem, and the technology is only suitable for solution spinning and is not suitable for a high-melting-point melt spinning process. Therefore, the development of the high-melting-point polyester thermal insulation fiber needs to design reasonable fiber matrix structure and composition according to the characteristics of functional materials, and challenges are presented to the regulation and control of the efficiency and structural relationship of the composite material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber, and provides a thought for preparing the polyester fiber which is uniform in dispersion of functional materials, high in photo-thermal conversion efficiency, environment-friendly, light in weight and capable of heat storage temperature regulation.
The aim of the invention can be achieved by the following technical scheme:
the invention relates to a preparation method of a skin-core type photo-thermal conversion-heat storage temperature regulation polyester fiber, which comprises the following steps:
s1: preparing carbon aerogel: preparing photo-thermal conversion cellulose-based aerogel based on nano-cellulose and photo-thermal conversion zirconium carbide nano-material, and carbonizing to obtain a composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material;
s2: and (3) hydrophobic modification: grinding the composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material prepared in the step S2, and performing surface hydrophobic modification to obtain hydrophobic-composite photo-thermal conversion carbon aerogel powder;
s3: and (3) preparing photo-thermal conversion carbon aerogel functional master batch: extruding and granulating the hydrophobic-composite photo-thermal conversion carbon aerogel powder obtained in the step S2 to obtain photo-thermal conversion carbon aerogel functional master batch;
s4: preparing PEG-PET solid-solid phase change master batch;
s5: co-extrusion spinning: extruding the photo-thermal conversion carbon aerogel functional master batch and the PEG-PET solid-solid phase change master batch, and spinning to obtain the skin-core type photo-thermal conversion-heat storage temperature adjustment polyester fiber.
Further, in S1, the preparation process specifically comprises: dispersing nano cellulose in an alkali solution, adding a photo-thermal conversion zirconium carbide nano material, mixing, stirring the mixed solution until the mixed solution is uniform, standing for degassing to obtain a homogeneous suspension, directionally freezing and drying the homogeneous suspension to obtain uniformly dispersed photo-thermal conversion cellulose-based aerogel, and carbonizing the photo-thermal conversion cellulose-based aerogel in a tube furnace to obtain the composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material.
Further, in S1, the mass fraction of cellulose in the mixed solution is 5-25%, preferably 10-20%, and the mass fraction of the photo-thermal material is 0.1-3%, preferably 1.5-2.5%;
s1, directional freezing time is 0.5-1h, freeze drying temperature is-80 ℃ to-18 ℃ and time is 24-48h;
stirring the mixed solution in a stirrer at the stirring speed of 1000-2000 r/min for 10-30 min, and standing for degassing for 12-24 h;
the carbonization treatment is carried out under the condition of nitrogen, the carbonization temperature is 400-700 ℃, the heat preservation time is 1-2 h, and the heating rate is 5-10 ℃/min.
Further, in S2, grinding the photo-thermal conversion carbon aerogel by adopting a nano grinder, and obtaining the composite cellulose-based carbon aerogel photo-thermal conversion powder with the particle size distribution of 100-300 nm through multistage grinding and screening;
immersing the composite cellulose-based carbon aerogel photo-thermal conversion powder in a silane coupling agent for surface hydrophobic modification, performing ultrasonic treatment at 60 ℃ for 1-2 h, and then filtering and drying at 80 ℃ to obtain the hydrophobic-composite photo-thermal conversion carbon aerogel powder.
Further, in S3, during the preparation process of the photo-thermal conversion carbon aerogel functional master batch: feeding the dried polyester chips into a double-screw extruder from a main feeding port, mixing by a melting screw, simultaneously adopting a side feeding method to pre-disperse and feed hydrophobic-composite photo-thermal conversion carbon aerogel powder into the double-screw extruder from the side direction through a turbine, mixing with a melted matrix melt, and obtaining the photo-thermal conversion carbon aerogel functional master batch through mixing melting, belt injection and granulating.
Further, in S3, the weight ratio of the polyester chip to the hydrophobic-composite photo-thermal conversion carbon aerogel powder is 55-75:25-45.
Further, in S4, the preparation process of the PEG-PET solid-solid phase change master batch comprises the following steps: mixing dimethyl terephthalate, glycol and a catalyst, adding the mixture into a reaction kettle, mixing, heating to 250 ℃, and stirring for esterification reaction for 3 hours;
then adding polyethylene glycol and a catalyst, heating to 300 ℃, reacting and polycondensing for 2-3 hours under vacuum, extruding the melt by a nozzle after the reaction is finished, and preparing PEG-PET solid-solid phase change master batch by water cooling, granulating and drying.
Further, in the S4, in the esterification reaction, the mass ratio of the dimethyl phthalate to the ethylene glycol to the catalyst antimony acetate is 5-35: 65-95: 0.03 to 0.05;
the mass ratio of polyethylene glycol to antimony acetate catalyst added in the polycondensation reaction is 25-55: 0.03 to 0.05.
Further, in S5, the process of co-extrusion spinning is: mixing the photo-thermal conversion thermal insulation master batch with polyester chips according to a preset proportion, feeding the mixture as a skin raw material into a double-screw extruder, feeding the PEG-PET solid-solid phase change functional material as a core layer into the screw extruder, respectively melting the skin and the core layer material through a spinning machine, accurately metering the materials through a metering pump, entering a spinning assembly, spraying the materials through a spinneret plate to form tows, pumping the tows through a monomer, cooling through lateral blowing, oiling in a bundling way, stretching and shaping, network interlacing, and then winding and shaping to obtain the skin-core thermal insulation polyester fiber with photo-thermal conversion/heat storage temperature regulation functions.
Further, the mass ratio of the raw materials of the skin layer and the core layer is 4:6, wherein the spinning temperature is 260-300 ℃ and the spinning speed is 800-3800 m/min.
The mechanism in S1-S5 in the technical scheme is explained as follows, which is convenient for the deep understanding of the person skilled in the art:
1) High dispersibility of zirconium carbide in aerogel: the surface of the nanocellulose is rich in hydroxyl groups, can form coordination with a plurality of transition metal ions, and can be used as a template for synthesizing one-dimensional semiconductor nanomaterial. Therefore, the nano-cellulose is used as a load substrate, and the natural polymer material is used as a bridge, so that zirconium carbide nano-particles can be effectively adsorbed and anchored to form the zirconium carbide and cellulose composite nano-material with a one-dimensional nano-structure, the aggregation of the zirconium carbide nano-particles is avoided, the dispersibility of the nano-cellulose and the zirconium carbide nano-particles is effectively improved, and the formed aerogel has high porosity, so that the photo-thermal conversion and heat preservation performance of the material are improved.
2) Support welding action of zirconium carbide in carbon aerogel: the photo-thermal conversion cellulose-based aerogel uses the nano cellulose as a load substrate of zirconium carbide, and the nano cellulose during carbonization is welded together by the zirconium carbide to reduce the polycondensation of cellulose during carbonization, so that the special porous structure of the carbon aerogel is maintained, and the nano-porosity and high porosity of the cellulose-based carbon aerogel are ensured.
3) Composite synergistic photo-thermal conversion material: the nano zirconium carbide is a photo-thermal material and has good light absorption capacity for visible light and near infrared light; cellulose is rich in a large amount of carbon elements, and cellulose-based carbon aerogel has high light absorptivity in the visible light and near infrared range. Meanwhile, the porous nano structure of the zirconium carbide/cellulose-based carbon aerogel can reduce the effective refractive index of the material and minimize the angle dependence of incident light, so that the effect of reducing light reflection is achieved; and the aperture acts as an optical microcavity, confining light by multiple light reflections and scattering, enhancing the interaction between light and material. Therefore, the material has strong light absorption capacity and light-heat conversion efficiency due to the synergistic effect of the inherent optical properties of the photo-thermal material and the multiple scattering/reflection of light in the micro-channel.
4) Hydrophobic modification of photothermal conversion nanopowder: the hydrophobic modification is carried out on the functional carbon aerogel particles, firstly, the hydrophobicity of the functional aerogel particles is improved, and the pores of the aerogel particles are ensured to be filled with dry air, so that the heat preservation performance of the material is improved; secondly, the dispersibility of the functional aerogel particles in the polymer matrix is improved, which is beneficial to improving the photo-thermal conversion performance of the material; and thirdly, after modification of aerogel particle powder, the combination property of the aerogel particle powder and a polymer matrix is improved, so that the spinnability and mechanical property of the fiber are improved.
5) Preparation of PEG-PET solid-solid phase change material: polyethylene glycol is used as a phase change component, and is subjected to polycondensation with dimethyl terephthalate and ethylene glycol to prepare the PEG-PET polymerization solid-solid phase change material, so that the leakage problem during the solid-liquid phase change of the polyethylene glycol is avoided, and the stability and durability of the phase change temperature regulating function of the fiber are improved.
Compared with the prior art, the invention has the following technical advantages:
1) The photo-thermal conversion thermal insulation material of the zirconium carbide/cellulose-based carbon aerogel prepared by the invention takes the nanocellulose as a photo-thermal material load substrate and is carbonized into the composite carbon aerogel to form the photo-thermal conversion material with the composite coordination type. The photo-thermal material has the advantages of strong light absorption capacity, high photo-thermal conversion efficiency, good heat retention performance, simple operation, low cost and environmental protection.
2) The sheath-core type photo-thermal conversion and heat storage temperature regulation polyester fiber prepared by the invention has higher photo-thermal conversion function and stable heat storage temperature regulation capability, and the high dispersibility of the functional powder in the polyester matrix reduces the influence of the addition of the functional material on the fiber production continuity and yarn quality, and improves the physical properties and production efficiency of the photo-thermal conversion heat storage thermal insulation fiber product.
3) The phase change enthalpy value of the prepared fiber reaches 14-16J/g; the xenon arc lamp is irradiated by a standard sunlight source for 10min, the temperature of the fabric is raised to 15 ℃, and the temperature difference duration is 15-17 min at 3 ℃.
Drawings
FIG. 1 is a diagram of a polyester fiber product prepared in example 1;
FIG. 2 is a view (magnified 1000 times) of the structure of a fiber cross section observed by a microscope in example 1.
Detailed Description
Aiming at the demands of the existing market and the technical problems existing in the prior art, the invention aims to provide a thought for preparing the polyester fiber which has the advantages of uniform dispersion of functional materials, high photo-thermal conversion efficiency, environment friendliness, light weight, heat storage and temperature regulation. Firstly, the nano-cellulose which is rich in hydroxyl groups on the surface and can form a fit with transition metal ions is selected as a load substrate, so that the nano-cellulose can effectively adsorb and anchor photo-thermal material zirconium carbide nano-particles, a one-dimensional semiconductor nano-material template is formed in the solution, and the dispersibility of the zirconium carbide particles in the nano-cellulose aerogel is effectively improved. Secondly, in order to solve the liquid-solid conversion in the phase change process of the phase change medium polyethylene glycol, the solid-solid phase change material is prepared by adopting the polymerization reaction of PEG-PET, so that the problem of leakage of the phase change material in melt spinning is avoided. The thermal insulation fiber with the skin-core structure is prepared by a double-screw extruder, and a novel method is provided for realizing development of the high-melting-point photo-thermal energy storage temperature regulation fiber.
The invention will now be described in detail with reference to the drawings and specific examples. In the technical scheme, the characteristics of preparation means, materials, structures or composition ratios and the like which are not explicitly described are regarded as common technical characteristics disclosed in the prior art.
Example 1
The skin-core type photo-thermal conversion and heat storage temperature regulation polyester fiber and the preparation method thereof provided in the embodiment comprise the following steps:
(1) preparation of photo-thermal conversion cellulose-based carbon aerogel: dispersing 10% nanocellulose in 0.01M alkali solution, and adding 1.5% photothermal conversion zirconium carbide nanomaterial (available from Shanghai super Wei nanotechnology limited Co., ltd.)For example, product lot 20220305001), the mixed solution was stirred until uniform, and the mixture was allowed to stand and deaerated to obtain a homogeneous suspension. After the homogeneous suspension is directionally frozen for 30min, the homogeneous suspension is transferred into an EYELA FDU-2110 freeze dryer and freeze-dried for 48h at the temperature of minus 80 ℃ to prepare the photo-thermal conversion cellulose-based aerogel with uniform dispersion. The aerogel was then placed in a tube furnace at N 2 Under the protection, the temperature rising rate of 5 ℃/min rises to 550 ℃, and the temperature is kept for 1h, so that the composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material is obtained.
(2) Hydrophobic modification of the composite carbon aerogel photo-thermal conversion powder: and (3) carrying out multistage grinding and screening on the composite photo-thermal conversion carbon aerogel obtained in the step (1) to obtain the photo-thermal conversion powder of the base carbon aerogel with the granularity of about 150 nm. Then KH-570 silane coupling agent is adopted to carry out surface hydrophobic modification, ultrasonic treatment is carried out for 1h, and the hydrophobic and composite photo-thermal conversion carbon aerogel powder is obtained after filtration and drying at 80 ℃.
(3) Preparing carbon aerogel photo-thermal conversion thermal master batch: feeding the dried polyester chips into a double-screw extruder from a main feeding port, feeding the composite photo-thermal conversion carbon aerogel powder prepared in the step (2) from the side direction, pre-dispersing at the speed of 100-300 rpm of a turbine, feeding the powder into the double-screw extruder, and carrying out melt mixing at 270 ℃, wherein the weight ratio of the polyester chips to the photo-thermal conversion aerogel powder is (3): 2, feeding; and then the master batch with the light-heat conversion and heat preservation functions is prepared through tape injection and grain cutting.
(4) PEG-PET solid-solid phase change master batch preparation: 385g of dimethyl terephthalate, 100ml of ethylene glycol and 10g of catalyst antimony acetate are mixed, added into a reaction kettle for mixing, heated to 250 ℃, stirred and esterified for 3 hours; then adding 192g of polyethylene glycol and 10g of catalyst antimony acetate, heating to 300 ℃, reacting and polycondensing for 2-3 h under vacuum, extruding the melt by a nozzle after the reaction is finished, and preparing PEG-PET phase change functional master batch by water cooling, granulating and drying.
(5) And (3) preparing the sheath-core type photo-thermal conversion and phase-change temperature-regulating polyester fiber: mixing the photo-thermal conversion carbon aerogel master batch with polyester chips according to a ratio of 1:4, mixing in proportion, and feeding the mixture serving as a cortex raw material into a double-screw extruder; feeding PEG-PET solid-solid phase change functional material as a core layer into a screw extruder, respectively melting the raw materials of the skin layer and the core layer by a spinning machine according to the proportion of 4:6, accurately metering by a metering pump, feeding the materials into a spinning component, and spraying the materials by a spinneret plate to form tows at the spinning temperature of 290 ℃; then the single body is pumped, the cross-air cooling is carried out, the cluster oiling is carried out, the stretching and shaping are carried out, and the network interlacing is carried out; and then winding and forming at 4000m/min to obtain the sheath-core type thermal insulation polyester fiber with photo-thermal conversion/heat storage and temperature adjustment, wherein the diagram of the obtained polyester fiber product is shown in figure 1, and corresponds to the structural diagram (magnified 1000 times) of the fiber cross section observed by a microscope.
Tests show that the phase change enthalpy value of the prepared fiber reaches 11-13J/g; the xenon arc lamp is irradiated by a standard sunlight source for 10min, the temperature of the fabric is raised to 12 ℃, and the temperature difference duration is 13-15 min at 3 ℃.
Example 2
The skin-core type photo-thermal conversion and heat storage temperature regulation polyester fiber and the preparation method thereof provided in the embodiment comprise the following steps:
(1) preparation of photo-thermal conversion cellulose-based carbon aerogel: dispersing 15% of nanocellulose in 0.01M alkali solution, adding 2% of photothermal conversion zirconium carbide nanomaterial (purchased from Shanghai super-Wei nanotechnology Co., ltd., product batch No. 20220305001), mixing, stirring to uniformity, standing, and degassing to obtain homogeneous suspension. After the homogeneous suspension is directionally frozen for 30min, the homogeneous suspension is transferred into an EYELA FDU-2110 freeze dryer and freeze-dried for 48h at the temperature of minus 80 ℃ to prepare the photo-thermal conversion cellulose-based aerogel with uniform dispersion. The aerogel was then placed in a tube furnace at N 2 Under the protection, the temperature rising rate of 5 ℃/min rises to 550 ℃, and the temperature is kept for 1h, so that the composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material is obtained.
(2) Hydrophobic modification of the composite carbon aerogel photo-thermal conversion powder: and (3) carrying out multistage grinding and screening on the composite photo-thermal conversion carbon aerogel obtained in the step (1) to obtain the photo-thermal conversion powder of the base carbon aerogel with the granularity of about 150 nm. Then KH-570 silane coupling agent is adopted to carry out surface hydrophobic modification, ultrasonic treatment is carried out for 1h, and the hydrophobic and composite photo-thermal conversion carbon aerogel powder is obtained after filtration and drying at 80 ℃.
(3) Preparing carbon aerogel photo-thermal conversion thermal master batch: feeding the dried polyester chips into a double-screw extruder from a main feeding port, feeding the composite photo-thermal conversion carbon aerogel powder prepared in the step (2) from the side direction, pre-dispersing at the speed of 100-300 rpm of a turbine, feeding the powder into the double-screw extruder, and carrying out melt mixing at 270 ℃, wherein the weight ratio of the polyester chips to the photo-thermal conversion aerogel powder is (3): 2, feeding; and then the master batch with the light-heat conversion and heat preservation functions is prepared through tape injection and grain cutting.
(4) PEG-PET solid-solid phase change master batch preparation: 385g of dimethyl terephthalate, 100ml of ethylene glycol and 10g of catalyst antimony acetate are mixed, added into a reaction kettle for mixing, heated to 250 ℃, stirred and esterified for 3 hours; then adding 192g of polyethylene glycol and 10g of catalyst antimony acetate, heating to 300 ℃, reacting and polycondensing for 2-3 h under vacuum, extruding the melt by a nozzle after the reaction is finished, and preparing PEG-PET phase change functional master batch by water cooling, granulating and drying.
(5) And (3) preparing the sheath-core type photo-thermal conversion and phase-change temperature-regulating polyester fiber: mixing the photo-thermal conversion carbon aerogel master batch with polyester chips according to a ratio of 1:4, mixing in proportion, and feeding the mixture serving as a cortex raw material into a double-screw extruder; feeding PEG-PET solid-solid phase change functional material as a core layer into a screw extruder, respectively melting the raw materials of the skin layer and the core layer by a spinning machine according to the proportion of 4:6, accurately metering by a metering pump, feeding the materials into a spinning component, and spraying the materials by a spinneret plate to form tows at the spinning temperature of 290 ℃; then the single body is pumped, the cross-air cooling is carried out, the cluster oiling is carried out, the stretching and shaping are carried out, and the network interlacing is carried out; and then winding and forming at 4000m/min to obtain the skin-core type thermal insulation polyester fiber with photo-thermal conversion/heat storage and temperature regulation functions.
Tests show that the phase change enthalpy value of the prepared fiber reaches 12-14J/g; the xenon arc lamp is irradiated by a standard sunlight source for 10min, the temperature of the fabric is raised to 14 ℃, and the temperature difference duration is 13-15 min at 3 ℃.
Example 3
The skin-core type photo-thermal conversion and heat storage temperature regulation polyester fiber and the preparation method thereof provided in the embodiment comprise the following steps:
(1) preparation of photo-thermal conversion cellulose-based carbon aerogel: dispersing 20% of nanocellulose in 0.01M alkali solution, and then adding 2.5% of photo-thermal conversion zirconium carbide nanomaterialPurchased from Shanghai super-Wei nanotechnology Co., ltd., product lot number 20220305001), and the mixed solution was stirred until uniform, and was left to stand for deaeration to obtain a homogeneous suspension. After the homogeneous suspension is directionally frozen for 30min, the homogeneous suspension is transferred into an EYELA FDU-2110 freeze dryer and freeze-dried for 48h at the temperature of minus 80 ℃ to prepare the photo-thermal conversion cellulose-based aerogel with uniform dispersion. The aerogel was then placed in a tube furnace at N 2 Under the protection, the temperature rising rate of 5 ℃/min rises to 550 ℃, and the temperature is kept for 1h, so that the composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material is obtained.
(2) Hydrophobic modification of the composite carbon aerogel photo-thermal conversion powder: and (3) carrying out multistage grinding and screening on the composite photo-thermal conversion carbon aerogel obtained in the step (1) to obtain the photo-thermal conversion powder of the base carbon aerogel with the granularity of about 150 nm. Then KH-570 silane coupling agent is adopted to carry out surface hydrophobic modification, ultrasonic treatment is carried out for 1h, and the hydrophobic and composite photo-thermal conversion carbon aerogel powder is obtained after filtration and drying at 80 ℃.
(3) Preparing carbon aerogel photo-thermal conversion thermal master batch: feeding the dried polyester chips into a double-screw extruder from a main feeding port, feeding the composite photo-thermal conversion carbon aerogel powder prepared in the step (2) from the side direction, pre-dispersing at the speed of 100-300 rpm of a turbine, feeding the powder into the double-screw extruder, and carrying out melt mixing at 270 ℃, wherein the weight ratio of the polyester chips to the photo-thermal conversion aerogel powder is (3): 2, feeding; and then the master batch with the light-heat conversion and heat preservation functions is prepared through tape injection and grain cutting.
(4) PEG-PET solid-solid phase change master batch preparation: 385g of dimethyl terephthalate, 100ml of ethylene glycol and 10g of catalyst antimony acetate are mixed, added into a reaction kettle for mixing, heated to 250 ℃, stirred and esterified for 3 hours; then adding 192g of polyethylene glycol and 10g of catalyst antimony acetate, heating to 300 ℃, reacting and polycondensing for 2-3 h under vacuum, extruding the melt by a nozzle after the reaction is finished, and preparing PEG-PET phase change functional master batch by water cooling, granulating and drying.
(5) And (3) preparing the sheath-core type photo-thermal conversion and phase-change temperature-regulating polyester fiber: mixing the photo-thermal conversion carbon aerogel master batch with polyester chips according to a ratio of 1:4, mixing in proportion, and feeding the mixture serving as a cortex raw material into a double-screw extruder; feeding PEG-PET solid-solid phase change functional material as a core layer into a screw extruder, respectively melting the raw materials of the skin layer and the core layer by a spinning machine according to the proportion of 4:6, accurately metering by a metering pump, feeding the materials into a spinning component, and spraying the materials by a spinneret plate to form tows at the spinning temperature of 290 ℃; then the single body is pumped, the cross-air cooling is carried out, the cluster oiling is carried out, the stretching and shaping are carried out, and the network interlacing is carried out; and then winding and forming at 4000m/min to obtain the skin-core type thermal insulation polyester fiber with photo-thermal conversion/heat storage and temperature regulation functions.
Tests show that the phase change enthalpy value of the prepared fiber reaches 14-16J/g; the xenon arc lamp is irradiated by a standard sunlight source for 10min, the temperature of the fabric is raised to 15 ℃, and the temperature difference duration is 15-17 min at 3 ℃.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. The preparation method of the sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber is characterized by comprising the following steps of:
s1: preparing carbon aerogel: preparing photo-thermal conversion cellulose-based aerogel based on nano-cellulose and photo-thermal conversion zirconium carbide nano-material, and carbonizing to obtain a composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material;
s2: and (3) hydrophobic modification: grinding the composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material prepared in the step S1, and performing surface hydrophobic modification to obtain hydrophobic-composite photo-thermal conversion carbon aerogel powder;
s3: and (3) preparing photo-thermal conversion carbon aerogel functional master batch: extruding and granulating the hydrophobic-composite photo-thermal conversion carbon aerogel powder obtained in the step S2 to obtain photo-thermal conversion carbon aerogel functional master batch;
s4: preparing PEG-PET solid-solid phase change master batch;
s5: co-extrusion spinning: mixing the photo-thermal conversion carbon aerogel functional master batch with polyester chips according to a preset proportion, feeding the mixture as a skin raw material into a double-screw extruder, feeding the PEG-PET solid-solid phase change functional material as a core layer into the screw extruder, and spinning to obtain the skin-core type photo-thermal conversion heat storage temperature regulation polyester fiber.
2. The preparation method of the sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber according to claim 1, wherein in the step S1, the preparation process is specifically as follows: dispersing nano cellulose in an alkali solution, adding a photo-thermal conversion zirconium carbide nano material, mixing, stirring the mixed solution until the mixed solution is uniform, standing for degassing to obtain a homogeneous suspension, directionally freezing and drying the homogeneous suspension to obtain uniformly dispersed photo-thermal conversion cellulose-based aerogel, and carbonizing the photo-thermal conversion cellulose-based aerogel in a tube furnace to obtain the composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material.
3. The preparation method of the sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber according to claim 2, wherein in S1, the mass fraction of cellulose in the mixed solution is 5-25%, and the mass fraction of photo-thermal material is 0.1-3%;
s1, directional freezing is carried out for 0.5-1h, the drying temperature is-80 ℃ to-18 ℃ and the time is 24-48h;
stirring the mixed solution in a stirrer at a stirring speed of 1000-2000 r/min for 10-30 min, and standing for degassing for 12-24 h;
the carbonization treatment is carried out under the nitrogen condition, the carbonization temperature is 400-700 ℃, the heat preservation time is 1-2 h, and the heating rate is 5-10 ℃/min.
4. The preparation method of the sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber is characterized in that in S2, a nano grinder is adopted to grind a composite zirconium carbide/cellulose-based carbon aerogel photo-thermal conversion material, and the composite cellulose-based carbon aerogel photo-thermal conversion powder with the particle size distribution of 100-300 nm is obtained through multistage grinding and screening;
immersing the composite cellulose-based carbon aerogel photo-thermal conversion powder in a silane coupling agent to carry out surface hydrophobic modification, carrying out ultrasonic treatment at 60 ℃ for 1-2 hours, and then filtering and drying at 80 ℃ to obtain the hydrophobic-composite photo-thermal conversion carbon aerogel powder.
5. The method for preparing the sheath-core type photo-thermal conversion-heat storage temperature adjustment polyester fiber according to claim 1, wherein in the step S3, in the preparation process of the photo-thermal conversion carbon aerogel functional master batch: feeding the dried polyester chips into a double-screw extruder from a main feeding port, mixing by a melting screw, simultaneously adopting a side feeding method to pre-disperse and feed hydrophobic-composite photo-thermal conversion carbon aerogel powder into the double-screw extruder from the side direction through a turbine, mixing with a melted matrix melt, and obtaining the photo-thermal conversion carbon aerogel functional master batch through mixing melting, belt injection and granulating.
6. The preparation method of the sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber according to claim 5, wherein in the step S3, the weight ratio of the polyester chip to the hydrophobic-composite photo-thermal conversion carbon aerogel powder is 55-75:25-45.
7. The preparation method of the sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber according to claim 1, wherein in the S4, the preparation process of the PEG-PET solid-solid phase change master batch is as follows: mixing dimethyl terephthalate, glycol and a catalyst, adding the mixture into a reaction kettle, mixing, heating to 250 ℃, and stirring for esterification reaction for 3 hours;
then adding polyethylene glycol and a catalyst, heating to 300 ℃, reacting and polycondensing for 2-3 hours under vacuum, extruding the melt by a nozzle after the reaction is finished, and performing water cooling, granulating and drying to obtain PEG-PET solid-solid phase change master batch.
8. The preparation method of the sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber according to claim 7, wherein in the S4, the mass ratio of dimethyl phthalate, ethylene glycol and catalyst antimony acetate in the esterification reaction is 5-35: 65-95: 0.03 to 0.05;
the mass ratio of polyethylene glycol to antimony acetate catalyst added in the polycondensation reaction is 25-55: 0.03 to 0.05.
9. The method for preparing the sheath-core type photo-thermal conversion-thermal storage temperature regulation polyester fiber according to claim 1, wherein in the step of S5, in the process of co-extrusion spinning: the skin and core materials are respectively melted by a spinning machine, accurately metered by a metering pump, enter a spinning component, are sprayed out by a spinneret plate to form tows, and are subjected to monomer suction, side blowing cooling, cluster oiling, stretching shaping, network interlacing, and winding shaping to obtain the skin-core type thermal insulation polyester fiber with the functions of photo-thermal conversion/heat storage and temperature regulation.
10. The preparation method of the sheath-core type photo-thermal conversion-heat storage temperature regulation polyester fiber according to claim 9, wherein the mass ratio of the raw materials of the sheath layer to the core layer is 4:6, wherein the spinning temperature is 260-300 ℃ and the spinning speed is 800-3800 m/min.
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