CN113235172A - Radiation refrigeration composite fiber and preparation method and application thereof - Google Patents
Radiation refrigeration composite fiber and preparation method and application thereof Download PDFInfo
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- CN113235172A CN113235172A CN202110440106.3A CN202110440106A CN113235172A CN 113235172 A CN113235172 A CN 113235172A CN 202110440106 A CN202110440106 A CN 202110440106A CN 113235172 A CN113235172 A CN 113235172A
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- composite fiber
- radiation refrigeration
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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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
Abstract
The invention discloses a radiation refrigeration composite fiber and a preparation method and application thereof. The radiation refrigeration composite fiber consists of matrix resin and acicular magnesium phosphite in a mass ratio of 9: 1-40: 1, and the preparation method comprises the following steps: 1) dispersing needle-shaped magnesium phosphite and matrix resin in a solvent to obtain spinning stock solution; 2) and adding the spinning solution into an electrostatic spinning machine, performing electrostatic spinning, and drying to obtain the radiation refrigeration composite fiber. The radiation refrigeration composite fiber has high infrared emissivity and high ultraviolet band reflectivity, is excellent in radiation refrigeration performance, good in ageing resistance and flexibility, simple in preparation process and suitable for large-scale mass production.
Description
Technical Field
The invention relates to the technical field of radiation refrigeration materials, in particular to radiation refrigeration composite fibers and a preparation method and application thereof.
Background
Radiation refrigeration is a novel refrigeration mode, has the characteristics of high efficiency and cleanness, and is expected to be used for refrigeration and cooling of urban buildings, outdoor facilities and the like. The radiation refrigeration material uses the space as a natural radiator, and radiates heat generated on the earth to the outer space through an atmospheric window, so that the material is required to have high short-wave-band reflectivity and medium infrared emissivity at the same time.
Currently, the materials reported in the literature for realizing radiation refrigeration mainly include photonic crystals (Raman a.p., Anoma m.a., Zhu l., et al.passive chemical below alloy direct below light [ J ] Nature,2014,515(7528): 540), porous polymer materials (manual J., Fu y., overview a.c., et al.high efficient porous polymer polymers copolymers for high efficient radiation chemical synthesis [ J ] Science,2018,362(6412): 315) and composite materials (Zhai y., Ma y., David s.n., zeylable chemical synthesis [ J ] Science,2018, 20112): 315) and composite materials (Zhai y., mac y., David s.n., zeylable chemical synthesis [ J ] spectrum-1062, 1067). The photonic crystal is assembled by depending on the particle effect aggregation of the nano particles, has high requirements on equipment and process, is difficult to realize large-scale mass production, and further cannot be put into practical application. The composite material superposed coating needs to accurately control the thickness of the coating, is not easy to form, can influence the tinting strength, tensile strength and the like of the material when the mass proportion of the inorganic particles is higher, and has poor practicability (Hontsunami and the like. coating chemistry, version 3. Beijing: scientific Press, 2019: 124-.
The inorganic powder such as silicon dioxide, aluminum phosphate, magnesium phosphite and the like belongs to inorganic radiation refrigeration powder with single component, can be used as pigment and filler to prepare radiation refrigeration coating with good performance, and has simple forming process and low cost. However, the inorganic radiation refrigeration powder has low refractive index, high mass addition ratio in the film forming process, reduced usage amount of film forming material, significantly increased cost, and reduced properties of wear resistance, leveling property, etc. (josip.m., sanja.l.b., marko.p., et al.infiluence of TiO2 and ZnO nanoparticles on properties of ceramic coated exposed surfaces, 2015,89:67-74), which need to be improved.
Disclosure of Invention
The invention aims to provide a radiation refrigeration composite fiber, and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
a radiation refrigeration composite fiber is composed of matrix resin and needle-shaped magnesium phosphite in a mass ratio of 9: 1-40: 1.
Preferably, the matrix resin is at least one of polyvinylidene fluoride (PVDF), Polystyrene (PS), polymethyl methacrylate (PMMA), Polyamide (PA), polyvinyl alcohol (PVA), Polyacrylonitrile (PAN), and polyvinyl pyrrolidone (PVP).
Preferably, the length of the needle-shaped magnesium phosphite is 0.2 to 2 μm.
Preferably, the diameter of the radiation refrigeration composite fiber is 0.8-2 μm.
The preparation method of the radiation refrigeration composite fiber comprises the following steps:
1) dispersing needle-shaped magnesium phosphite and matrix resin in a solvent to obtain spinning stock solution;
2) and adding the spinning solution into an electrostatic spinning machine, performing electrostatic spinning, and drying to obtain the radiation refrigeration composite fiber.
Preferably, the solvent in step 1) is at least one of N, N-Dimethylformamide (DMF), acetone, dichloromethane and xylene.
Preferably, the total mass of the needle-like magnesium phosphite and the matrix resin in the step 1) accounts for 10-50% of the mass of the solvent.
Preferably, the electrostatic spinning in the step 2) has the working voltage of 13kV to 16kV, the polar plate distance of 10cm to 15cm and the extrusion speed of 0.015mm/s to 0.09 mm/s.
More preferably, the electrostatic spinning in the step 2) has the working voltage of 13kV to 16kV, the polar plate distance of 13cm to 15cm and the extrusion speed of 0.03mm/s to 0.07 mm/s.
Preferably, the electrostatic spinning in the step 2) is carried out under the condition that the relative humidity of the environment is 45% -60%.
More preferably, the electrostatic spinning in step 2) is performed under the condition that the relative humidity of the environment is 50% to 60%.
Preferably, the drying in step 2) is carried out at 60 ℃ to 105 ℃.
The invention has the beneficial effects that: the radiation refrigeration composite fiber has high infrared emissivity and high ultraviolet band reflectivity, is excellent in radiation refrigeration performance, good in ageing resistance and flexibility, simple in preparation process and suitable for large-scale mass production.
Specifically, the method comprises the following steps:
1) the radiation refrigeration composite fiber has low addition amount of needle-shaped magnesium phosphite, but has excellent radiation refrigeration performance, and compared with the traditional coating which can realize better radiation refrigeration effect only by adding 40-50 wt% of inorganic radiation refrigeration powder, the radiation refrigeration composite fiber has simpler operation and stronger practicability;
2) the acicular structure of the acicular magnesium phosphite in the radiation refrigeration composite fiber meets Rayleigh scattering conditions, can effectively reflect solar rays in an ultraviolet band, improve the light aging resistance of the composite fiber, obviously improve the reflectivity of a short band of the composite fiber, and is induced by the acicular magnesium phosphite
The composite fiber with the mass ratio of low inorganic radiation refrigeration powder can minimize the absorption of solar radiation and has stronger heat dissipation capacity and better refrigeration effect;
3) the radiation refrigeration composite fiber can be used for manufacturing outdoor fabrics with radiation refrigeration effects, such as tents, sunshade umbrellas and the like, can also be used for manufacturing clothing fibers, fiber reinforced plastics and the like, and has strong practicability.
Drawings
FIG. 1 is an SEM image of acicular magnesium phosphite in example 2.
Fig. 2 is a TEM image of the radiation-cooled composite fiber of example 2.
FIG. 3 is an SEM image of the radiation refrigerating composite fibers of examples 1 to 3.
FIG. 4 is a reflectance curve of the radiation refrigeration composite fibers of examples 1 to 3 and the PVDF fiber of the comparative example.
FIG. 5 is a graph showing emissivity curves of the radiation refrigeration composite fibers of examples 1 to 3 and the PVDF fiber of the comparative example.
FIG. 6 is a graph showing emissivity curves of the radiation refrigeration composite fibers of examples 3 to 6.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Note: the needle-like magnesium phosphite in the embodiments 1-6 is synthesized by a hydrothermal method, and the specific synthesis steps are as follows: adding 0.02mol of solid phosphorous acid and 0.02mol of tetrahydrate magnesium acetate into a beaker, adding a proper amount of deionized water, placing the beaker on a magnetic stirrer, stirring to obtain a clear solution, dropwise adding a sodium hydroxide solution while stirring, simultaneously controlling the pH value of the solution to be 7-10 in real time by using a pH meter, sealing the beaker by using a preservative film after the sodium hydroxide solution is completely added, aging for 30min, transferring the solution into a reaction kettle with a polytetrafluoroethylene lining, transferring the reaction kettle into an oven, reacting for 24h at 180 ℃, performing suction filtration and washing on a reaction product for multiple times, placing the reaction product into the oven, and drying for 4h at 105 ℃ to obtain the acicular magnesium phosphite.
Example 1:
a radiation refrigeration composite fiber is prepared by the following steps:
1) adding 0.055g of needle-shaped magnesium phosphite with the length of 0.5-2 mu m and 2.2g of PVDF powder with the number average molecular weight of 320000 into 10g of DMF, and stirring for 6 hours to obtain spinning stock solution;
2) and (2) adding the spinning solution into an electrostatic spinning machine, setting the distance between polar plates to be 13cm, setting the working voltage to be 13 kV-15 kV, setting the extrusion speed to be 0.045mm/s and the relative humidity of the environment to be 55%, carrying out electrostatic spinning, collecting the fibers on an aluminum foil by adopting a flat plate method, and drying at 95 ℃ to obtain the radiation refrigeration composite fiber.
Example 2:
a radiation refrigeration composite fiber is prepared by the following steps:
1) adding 0.11g of needle-shaped magnesium phosphite with the length of 0.5-2 mu m and 2.2g of PVDF powder with the number average molecular weight of 320000 into 10g of DMF, and stirring for 6 hours to obtain spinning stock solution;
2) and (2) adding the spinning solution into an electrostatic spinning machine, setting the distance between polar plates to be 13cm, setting the working voltage to be 13 kV-15 kV, setting the extrusion speed to be 0.045mm/s and the relative humidity of the environment to be 55%, carrying out electrostatic spinning, collecting the fibers on an aluminum foil by adopting a flat plate method, and drying at 80 ℃ to obtain the radiation refrigeration composite fiber.
Example 3:
a radiation refrigeration composite fiber is prepared by the following steps:
1) adding 0.165g of needle-shaped magnesium phosphite with the length of 0.5-2 mu m and 2.2g of PVDF powder with the number average molecular weight of 320000 into 10g of DMF, and stirring for 6 hours to obtain spinning stock solution;
2) and (2) adding the spinning solution into an electrostatic spinning machine, setting the distance between polar plates to be 13cm, setting the working voltage to be 13 kV-15 kV, setting the extrusion speed to be 0.045mm/s and the relative humidity of the environment to be 55%, carrying out electrostatic spinning, collecting the fibers on an aluminum foil by adopting a flat plate method, and drying at 80 ℃ to obtain the radiation refrigeration composite fiber.
Example 4:
a radiation refrigeration composite fiber is prepared by the following steps:
1) adding 0.165g of needle-shaped magnesium phosphite with the length of 0.5-2 mu m and 4.2g of PVP powder with the number average molecular weight of 120000 into 10g of DMF, and stirring for 6 hours to obtain spinning stock solution;
2) and (2) adding the spinning solution into an electrostatic spinning machine, setting the distance between polar plates to be 13cm, setting the working voltage to be 13 kV-15 kV, setting the extrusion speed to be 0.045mm/s and the relative humidity of the environment to be 55%, carrying out electrostatic spinning, collecting the fibers on an aluminum foil by adopting a flat plate method, and drying at 80 ℃ to obtain the radiation refrigeration composite fiber.
Example 5:
a radiation refrigeration composite fiber is prepared by the following steps:
1) adding 0.165g of needle-shaped magnesium phosphite with the length of 0.5-2 mu m and 4.0g of PMMA block with the number average molecular weight of 200000 into 10g of DMF, and stirring for 6 hours to obtain spinning stock solution;
2) and (2) adding the spinning solution into an electrostatic spinning machine, setting the distance between polar plates to be 13cm, setting the working voltage to be 13 kV-15 kV, setting the extrusion speed to be 0.045mm/s and the relative humidity of the environment to be 55%, carrying out electrostatic spinning, collecting the fibers on an aluminum foil by adopting a flat plate method, and drying at 80 ℃ to obtain the radiation refrigeration composite fiber.
Example 6:
a radiation refrigeration composite fiber is prepared by the following steps:
1) adding 0.165g of needle-shaped magnesium phosphite with the length of 0.5-2 mu m and 1.6g of PS block with the number average molecular weight of 400000 into 10g of DMF, and stirring for 6 hours to obtain spinning solution;
2) and (2) adding the spinning solution into an electrostatic spinning machine, setting the distance between polar plates to be 13cm, setting the working voltage to be 13 kV-15 kV, setting the extrusion speed to be 0.045mm/s and the relative humidity of the environment to be 55%, carrying out electrostatic spinning, collecting the fibers on an aluminum foil by adopting a flat plate method, and drying at 80 ℃ to obtain the radiation refrigeration composite fiber.
Comparative example:
a PVDF fiber, its preparation method includes the following steps:
1) 2.2g of PVDF powder with the number average molecular weight of 320000 is added into 10g of DMF and stirred for 6 hours to obtain spinning solution;
2) and (2) adding the spinning solution into an electrostatic spinning machine, setting the distance between polar plates to be 13cm, setting the working voltage to be 13 kV-15 kV, setting the extrusion rate to be 0.045mm/s and the relative humidity of the environment to be 55%, carrying out electrostatic spinning, collecting the fibers on an aluminum foil by adopting a flat plate method, and drying at 95 ℃ to obtain the PVDF fibers.
And (3) performance testing:
1) the Scanning Electron Microscope (SEM) image of acicular magnesium phosphite in example 2 is shown in fig. 1, the Transmission Electron Microscope (TEM) image of the radiation refrigeration composite fiber in example 2 is shown in fig. 2, and the SEM image of the radiation refrigeration composite fibers in examples 1 to 3 is shown in fig. 3 (in the figures, a to c are the radiation refrigeration composite fibers in examples 1 to 3 in order).
As can be seen from fig. 1: the length of the needle-shaped magnesium phosphite is 0.5-2 mu m.
As can be seen from fig. 2: the needle-shaped magnesium phosphite can be well embedded in the radiation refrigeration composite fiber.
As can be seen from fig. 3: the diameter of the radiation refrigeration composite fiber is 0.8-2 μm.
2) The reflectance curves of the radiation refrigeration composite fibers of examples 1-3 and the PVDF fibers of the comparative example are shown in FIG. 4.
As can be seen from fig. 4: the average solar spectrum (300nm to 2500nm) reflectivities of the radiation refrigeration composite fibers of examples 1 to 3 and the PVDF fibers of the comparative examples are 95.53%, 99.18%, 96.56% and 85.91% in sequence, which shows that the needle-like morphology of the needle-like magnesium phosphite is benefited, and the Rayleigh scattering condition is satisfied, so that the ultraviolet band reflection performance of the PVDF fibers can be remarkably improved, and the visible light and near infrared reflection performance can be enhanced due to the high reflectivity of the needle-like magnesium phosphite.
3) Emissivity curves of the radiation refrigeration composite fibers of examples 1 to 3 and the PVDF fiber of the comparative example are shown in fig. 5.
As can be seen from fig. 5: the emissivity of the radiation refrigeration composite fibers of examples 1-3 and the PVDF fibers of the comparative example are 89.6%, 88.7%, 90.9% and 74.8% in the order of 8-13 μm, which illustrates that the high-order PVDF fibers benefit from the sudden change excitation of the refractive index at the boundary between the P-O, Mg-O bond and the inorganic microsphere in various chemical environments of acicular magnesium phosphite
And resonance is realized, so that the emissivity is greatly improved under the condition of low inorganic radiation refrigeration powder content.
4) The emissivity curves of the radiation refrigeration composite fibers of examples 3-6 are shown in FIG. 6.
As can be seen from fig. 6: the fibers obtained by compounding different matrix resins and the needle-shaped magnesium phosphite and carrying out electrostatic spinning have higher emissivity, and in an atmospheric window, the emissivity of the PMMA composite fiber reaches 90.27%, and the emissivity of the PS composite fiber reaches 91.06%.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The radiation refrigeration composite fiber is characterized by comprising matrix resin and needle-shaped magnesium phosphite in a mass ratio of 9: 1-40: 1.
2. The radiation-cooled composite fiber of claim 1, wherein: the matrix resin is at least one of polyvinylidene fluoride, polystyrene, polymethyl methacrylate, polyamide, polyvinyl alcohol, polyacrylonitrile and polyvinylpyrrolidone.
3. A radiation refrigerating composite fibre according to claim 1 or 2, characterised in that: the length of the needle-shaped magnesium phosphite is 0.2-2 mu m.
4. A radiation refrigerating composite fibre according to claim 1 or 2, characterised in that: the diameter of the radiation refrigeration composite fiber is 0.8-2 μm.
5. The preparation method of the radiation refrigeration composite fiber according to any one of claims 1 to 4, characterized by comprising the following steps:
1) dispersing needle-shaped magnesium phosphite and matrix resin in a solvent to obtain spinning stock solution;
2) and adding the spinning solution into an electrostatic spinning machine, performing electrostatic spinning, and drying to obtain the radiation refrigeration composite fiber.
6. The method for preparing a radiation refrigerating composite fiber according to claim 5, wherein: the solvent in the step 1) is at least one of N, N-dimethylformamide, acetone, dichloromethane and xylene.
7. The method for producing a radiation refrigerating composite fiber according to claim 5 or 6, characterized in that: the total mass of the needle-like magnesium phosphite and the matrix resin in the step 1) accounts for 10-50% of the mass of the solvent.
8. The method for preparing a radiation refrigerating composite fiber according to claim 5, wherein: the working voltage of the electrostatic spinning in the step 2) is 13 kV-16 kV, the distance between the polar plates is 10 cm-15 cm, and the extrusion speed is 0.015 mm/s-0.09 mm/s.
9. The method for producing a radiation refrigerating composite fiber according to claim 5 or 8, characterized in that: and 2) carrying out electrostatic spinning under the condition that the relative humidity of the environment is 45-60%.
10. Use of the radiation refrigeration composite fiber according to any one of claims 1 to 4 in the preparation of a radiation refrigeration material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113827079A (en) * | 2021-09-29 | 2021-12-24 | 浙江真爱毯业科技有限公司 | Outdoor blanket with day radiation refrigeration function |
| CN114293320A (en) * | 2022-01-10 | 2022-04-08 | 上海交通大学 | High-heat-dissipation radiation cooling film for high-power heating device and preparation method thereof |
| CN114659290A (en) * | 2022-03-23 | 2022-06-24 | 国家纳米科学中心 | Fiber array-based radiation refrigeration surface and preparation method and application thereof |
| CN115323626A (en) * | 2022-08-30 | 2022-11-11 | 暨南大学 | Polymer and functional complex composite thermal management material and preparation method and application thereof |
| CN115652463A (en) * | 2022-10-18 | 2023-01-31 | 清华大学 | Application of polyformaldehyde fiber in indoor and outdoor environment human body radiation refrigeration |
| CN115652463B (en) * | 2022-10-18 | 2024-04-30 | 清华大学 | Application of polyoxymethylene fiber in human body radiation refrigeration in indoor and outdoor environments |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113827079A (en) * | 2021-09-29 | 2021-12-24 | 浙江真爱毯业科技有限公司 | Outdoor blanket with day radiation refrigeration function |
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| CN115652463A (en) * | 2022-10-18 | 2023-01-31 | 清华大学 | Application of polyformaldehyde fiber in indoor and outdoor environment human body radiation refrigeration |
| CN115652463B (en) * | 2022-10-18 | 2024-04-30 | 清华大学 | Application of polyoxymethylene fiber in human body radiation refrigeration in indoor and outdoor environments |
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Application publication date: 20210810 |