CN117385485A - Rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber and preparation method and application thereof - Google Patents
Rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber and preparation method and application thereof Download PDFInfo
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- CN117385485A CN117385485A CN202311667086.9A CN202311667086A CN117385485A CN 117385485 A CN117385485 A CN 117385485A CN 202311667086 A CN202311667086 A CN 202311667086A CN 117385485 A CN117385485 A CN 117385485A
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- Prior art keywords
- rare earth
- phosphate
- passive cooling
- silicate
- broad spectrum
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Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 173
- 238000001816 cooling Methods 0.000 title claims abstract description 104
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 103
- 239000000835 fiber Substances 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000004744 fabric Substances 0.000 claims abstract description 60
- 238000009413 insulation Methods 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 9
- -1 rare earth compound Chemical class 0.000 claims description 92
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 62
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 53
- 239000004408 titanium dioxide Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000001354 calcination Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 23
- 239000002002 slurry Substances 0.000 claims description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 21
- 239000002131 composite material Substances 0.000 claims description 19
- 229910019142 PO4 Inorganic materials 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- JCFISKANHFQUCT-UHFFFAOYSA-N [Y].[La] Chemical compound [Y].[La] JCFISKANHFQUCT-UHFFFAOYSA-N 0.000 claims description 18
- LQFNMFDUAPEJRY-UHFFFAOYSA-K lanthanum(3+);phosphate Chemical compound [La+3].[O-]P([O-])([O-])=O LQFNMFDUAPEJRY-UHFFFAOYSA-K 0.000 claims description 18
- 239000010452 phosphate Substances 0.000 claims description 18
- 239000003963 antioxidant agent Substances 0.000 claims description 16
- 230000003078 antioxidant effect Effects 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 13
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 13
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 13
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 10
- 239000004753 textile Substances 0.000 claims description 9
- 229910017569 La2(CO3)3 Inorganic materials 0.000 claims description 8
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 claims description 8
- 229960001633 lanthanum carbonate Drugs 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004576 sand Substances 0.000 claims description 7
- 238000010008 shearing Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 238000009987 spinning Methods 0.000 claims description 6
- QVOIJBIQBYRBCF-UHFFFAOYSA-H yttrium(3+);tricarbonate Chemical compound [Y+3].[Y+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O QVOIJBIQBYRBCF-UHFFFAOYSA-H 0.000 claims description 6
- IOVBQFVGIMLIRA-UHFFFAOYSA-H cerium(3+) lanthanum(3+) diphosphate Chemical compound [La+3].[Ce+3].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O IOVBQFVGIMLIRA-UHFFFAOYSA-H 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- KJNZTHUWRRLWOA-UHFFFAOYSA-K europium(3+);phosphate Chemical compound [Eu+3].[O-]P([O-])([O-])=O KJNZTHUWRRLWOA-UHFFFAOYSA-K 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 5
- BJRVEOKYZKROCC-UHFFFAOYSA-K samarium(3+);phosphate Chemical compound [Sm+3].[O-]P([O-])([O-])=O BJRVEOKYZKROCC-UHFFFAOYSA-K 0.000 claims description 5
- 239000001038 titanium pigment Substances 0.000 claims description 5
- SJYRPJPOXAEUIL-UHFFFAOYSA-N [La].[Gd] Chemical compound [La].[Gd] SJYRPJPOXAEUIL-UHFFFAOYSA-N 0.000 claims description 4
- LENJPRSQISBMDN-UHFFFAOYSA-N [Y].[Ce] Chemical compound [Y].[Ce] LENJPRSQISBMDN-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- OYJCSRLEYSNWPB-UHFFFAOYSA-H cerium(3+) yttrium(3+) diphosphate Chemical compound [Ce+3].P(=O)([O-])([O-])[O-].[Y+3].P(=O)([O-])([O-])[O-] OYJCSRLEYSNWPB-UHFFFAOYSA-H 0.000 claims description 4
- TYAVIWGEVOBWDZ-UHFFFAOYSA-K cerium(3+);phosphate Chemical compound [Ce+3].[O-]P([O-])([O-])=O TYAVIWGEVOBWDZ-UHFFFAOYSA-K 0.000 claims description 4
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- XFULIUKARWFBDF-UHFFFAOYSA-K erbium(3+);phosphate Chemical compound [Er+3].[O-]P([O-])([O-])=O XFULIUKARWFBDF-UHFFFAOYSA-K 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- ZFEZZRFBMNCXLQ-UHFFFAOYSA-K holmium(3+);phosphate Chemical compound [Ho+3].[O-]P([O-])([O-])=O ZFEZZRFBMNCXLQ-UHFFFAOYSA-K 0.000 claims description 4
- 238000002074 melt spinning Methods 0.000 claims description 4
- 229920002635 polyurethane Polymers 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- YXNVQKRHARCEKL-UHFFFAOYSA-K ytterbium(3+);phosphate Chemical compound [Yb+3].[O-]P([O-])([O-])=O YXNVQKRHARCEKL-UHFFFAOYSA-K 0.000 claims description 4
- 229910000164 yttrium(III) phosphate Inorganic materials 0.000 claims description 4
- UXBZSSBXGPYSIL-UHFFFAOYSA-K yttrium(iii) phosphate Chemical compound [Y+3].[O-]P([O-])([O-])=O UXBZSSBXGPYSIL-UHFFFAOYSA-K 0.000 claims description 4
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 3
- WMOHXRDWCVHXGS-UHFFFAOYSA-N [La].[Ce] Chemical compound [La].[Ce] WMOHXRDWCVHXGS-UHFFFAOYSA-N 0.000 claims description 3
- GNKHOVDJZALMGA-UHFFFAOYSA-N [Y].[Zr] Chemical compound [Y].[Zr] GNKHOVDJZALMGA-UHFFFAOYSA-N 0.000 claims description 3
- JAOZQVJVXQKQAD-UHFFFAOYSA-K gadolinium(3+);phosphate Chemical compound [Gd+3].[O-]P([O-])([O-])=O JAOZQVJVXQKQAD-UHFFFAOYSA-K 0.000 claims description 3
- RQXZRSYWGRRGCD-UHFFFAOYSA-H gadolinium(3+);tricarbonate Chemical compound [Gd+3].[Gd+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O RQXZRSYWGRRGCD-UHFFFAOYSA-H 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- AZJLMWQBMKNUKB-UHFFFAOYSA-N [Zr].[La] Chemical compound [Zr].[La] AZJLMWQBMKNUKB-UHFFFAOYSA-N 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 2
- 239000004626 polylactic acid Substances 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 35
- 235000010215 titanium dioxide Nutrition 0.000 description 30
- 238000009940 knitting Methods 0.000 description 21
- 239000006087 Silane Coupling Agent Substances 0.000 description 19
- 230000000694 effects Effects 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 8
- 229920001778 nylon Polymers 0.000 description 7
- 238000002310 reflectometry Methods 0.000 description 6
- 238000005057 refrigeration Methods 0.000 description 6
- 229920000728 polyester Polymers 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009323 psychological health Effects 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a rare earth-based broad spectrum passive cooling hollow heat-insulating fiber, a preparation method and application thereof, wherein the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber comprises the following components in parts by weight: 0.1% -10% of rare earth passive cooling powder; 85% -95% of base material powder; 1% -10% of an auxiliary agent. The fiber has excellent cooling and heat insulation performance, and after the simulated light source irradiates 0.5 to h, the temperature of the fabric covering part woven by the fiber is lower than that of the common fabric covering part by more than 2.5 degrees.
Description
Technical Field
The invention belongs to the technical field of textile weaving, and particularly relates to a rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber, and a preparation method and application thereof.
Background
The hot environment in summer also brings a certain health threat while affecting the living comfort of people. Textiles provide a protective barrier for the body and play a critical role in the heat exchange between the individual and the environment. The textile is endowed with a certain cooling function by introducing functional components, improving weaving technology and the like, and the cooling fabric is utilized to promote the thermal comfort of the human body and the local microenvironment around the human body in a hot environment, so that the textile has important significance for maintaining the physical and psychological health of the human body and reducing the building energy consumption brought by a heating ventilation air conditioning system.
The cooling fabric can be divided into two types, namely an active cooling fabric and a passive cooling fabric by a cooling principle. The active cooling fabric adjusts the temperature of a human body by means of energy conversion, intelligent sensing, phase-change refrigeration and the like, has obvious refrigeration effect, but has the problems of great technical difficulty, immature process, noise in use, incapability of washing with water, poor practicability and the like, and is difficult to directly apply in industrialization. Passive cooling is mainly achieved from the following two aspects: (1) The absorption and the emissivity of the fabric to the radiation of the human body are increased, and the skin of the human body has high heat radiation in the far infrared band of 7-14 mu m; (2) In summer, a large part of heat radiation comes from the sun, the reflectivity of the fabric to sunlight in the wavelength range of 300-2500 nm is improved, the temperature of the fabric can be reduced, the conduction of environmental heat to the skin surface is further reduced, and the purposes of cooling and heat insulation are achieved. At present, a passive cooling fabric is also in a development research stage, and the radiation refrigeration fabric has the advantages of complex preparation process, higher cost and poor cooling effect; near infrared band energy accounts for more than 55% of solar energy, while most fabrics have lower near infrared reflectivity, and only white fabrics capable of reflecting visible light have better reflection cooling effect; the heat conductivity coefficient of the conventional passive cooling materials such as titanium dioxide, aluminum oxide and the like is high, and the heat insulation performance of the fabric is poor.
Disclosure of Invention
In view of the above, the invention aims to overcome the defects in the prior art and provides a rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber, and a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
the invention provides a rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber, which comprises the following components in percentage by weight:
0.1% -10% of rare earth passive cooling powder;
85% -95% of base material powder;
1% -10% of an auxiliary agent;
wherein, the rare earth passive cooling powder comprises the following components in percentage by weight: 50-70% of reflective rare earth compound and 30-50% of rare earth compound silicate;
the reflective rare earth compound is obtained by calcining rare earth phosphate, titanium dioxide and aluminum oxide together; the rare earth composite silicate comprises one or more than two of lanthanum cerium silicate, lanthanum yttrium silicate, yttrium cerium silicate, zirconium lanthanum silicate, zirconium yttrium silicate and lanthanum gadolinium silicate.
Preferably, the mass ratio of the rare earth phosphate, the titanium dioxide and the aluminum oxide in the reflective rare earth compound is 1: (0.5-2): (0.1-1).
Preferably, the rare earth phosphate comprises one or more of lanthanum phosphate, cerium phosphate, yttrium phosphate, gadolinium phosphate, samarium phosphate, ytterbium phosphate, europium phosphate, holmium phosphate, erbium phosphate, lanthanum cerium phosphate and yttrium cerium phosphate.
Preferably, the substrate powder is one or more of polyethylene, polypropylene, polyethylene terephthalate, polylactic acid, polyacrylonitrile, polyamide, ethylene-octene copolymer, polybutylene terephthalate, polypropylene terephthalate, polyurethane and polyvinyl alcohol.
Preferably, the auxiliary agent is one or more of dispersing agent, antioxidant, slipping agent and release agent.
Preferably, the preparation method of the reflective rare earth compound comprises the following steps:
(1) Uniformly dispersing 4N-level rare earth carbonate into deionized water at 80-100 ℃ with the concentration of 50-500 g/L, slowly dropwise adding phosphoric acid into the deionized water under mechanical stirring at the rotation speed of 200 r/min-1000 r/min until no bubbles are generated in the solution, adding a pH regulator to adjust the pH to be neutral, carrying out suction filtration and drying, and obtaining rare earth phosphate at the drying temperature of 90-110 ℃;
(2) And (3) uniformly mixing the rare earth phosphate obtained in the step (1) with titanium pigment and aluminum oxide by a solid-phase high-speed mixer, and placing the mixture into a muffle furnace for calcination at 900-1600 ℃ to obtain the reflective rare earth compound.
Preferably, the preparation method of the rare earth composite silicate comprises the following steps:
uniformly dispersing the first carbonate, the second carbonate and the silicon oxide in deionized water, wherein the solid content is 30% -80%, placing the obtained dispersion in a ball mill, ball-milling for 12-24 hours at a rotating speed of 200-500 r/min, carrying out suction filtration and drying, wherein the drying temperature is 90-110 ℃, calcining in a muffle furnace, taking out, carrying out secondary ball milling at a rotating speed of 200-500 r/min, wherein the ball-milling solid content is 30% -80%, the ball-milling time is 12-24 hours, and carrying out suction filtration and drying, and the drying temperature is 90-110 ℃, thus obtaining the rare earth composite silicate;
the first carbonate and the second carbonate are different and are respectively and independently selected from one of lanthanum carbonate, cerium carbonate, zirconium carbonate, yttrium carbonate and gadolinium carbonate.
Further preferably, the molar ratio of the first carbonate, the second carbonate to the silicon oxide is 1:1:1.
the second aspect of the invention provides a preparation method of the rare earth-based broad spectrum passive cooling hollow heat insulation fiber, which comprises the following steps:
(1) Pre-dispersing the reflective rare earth compound, rare earth compound silicate and an auxiliary agent in deionized water, uniformly mixing, shearing and dispersing at a high speed by a sand mill for 0.5-10 h, obtaining rare earth passive cooling nano slurry with the particle size distribution of 100-800 nm, concentrating the nano slurry by concentrating under reduced pressure and removing water, dispersing base material powder into concentrated slurry, adding the auxiliary agent, and uniformly mixing by a high-speed mixer to obtain a mixture;
(2) Drying the mixture obtained in the step (1) at 100-130 ℃, carrying out melt extrusion granulation at a melting temperature of 150-350 ℃ and an extrusion speed of 100-300 r/min and a granulating speed of 10-30 m/min, and obtaining rare earth-based broad spectrum cooling heat insulation master batch;
(3) And (3) drying the rare earth-based broad spectrum cooling heat-insulating master batch obtained in the step (2), and preparing the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber by using an annular hollow spinneret plate through a melt spinning process after the water content is lower than 200 ppm, wherein the spinning temperature is 150-350 ℃, and the winding speed is 1800-5000 m/min.
The third aspect of the invention also provides application of the rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber in the field of textile products such as clothing fabrics, home textiles, industrial textiles and outdoor fabrics.
Compared with the prior art, the invention has the following advantages:
(1) In the rare earth passive cooling powder, the titanium dioxide has high reflection performance in the visible light-near infrared range of 300-1000 nm, the rare earth phosphate has high reflection capability in the near infrared range of 1000 nm-2500 nm, and the titanium dioxide and the rare earth phosphate can endow the fabric with excellent visible-near infrared reflection performance after being mixed and calcined. Meanwhile, the aluminum oxide has higher visible-near infrared reflection performance and a compact surface, and the compact and smooth surface is beneficial to improving the reflectivity of the small-particle-size nano particles. The three components are calcined together, so that defects in the material are reduced, the absorption of the material is inhibited, and the obtained reflective rare earth compound has excellent visible-near infrared reflection performance in the range of 300 nm-2500 nm, and can reflect more than 85% of sunlight heat.
(2) The rare earth composite silicate in the rare earth passive cooling powder combines the high emission properties of two metal elements and silicon element, and the far infrared emissivity of the rare earth composite silicate in an atmosphere window of 8-13 mu m is more than 0.95, so that the purposes of passive refrigeration and low energy consumption refrigeration are achieved; the thermal conductivity of rare earth silicate at normal temperature is about 1.5W/(m.K), and compared with other passive cooling materials, the rare earth silicate has better heat insulation effect.
(3) Compared with the common fiber, the hollow heat-insulating fiber has lower heat conductivity and better heat-insulating property, and can improve the heat-insulating capability of the fiber in hot environments.
(4) The reflective rare earth compound and rare earth compound silicate in the invention act together, and the hollow structure of the fiber is combined, so that the rare earth-based broad-spectrum passive cooling hollow heat insulation fiber has excellent cooling heat insulation performance, and after the simulated light source irradiates 0.5 h, the temperature of the fabric covering part woven by the fiber is lower than that of the common fabric covering part by more than 2.5 ℃.
(5) The hollow heat-insulating fiber has simple preparation process and is easy for large-scale production.
Drawings
FIG. 1 is a schematic cooling diagram of a rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric;
FIG. 2 is an XRD spectrum of lanthanum phosphate;
FIG. 3 is an XRD spectrum of a reflective rare earth composite;
FIG. 4 is an XRD spectrum of a rare earth complex silicate;
FIG. 5 is a reflectance spectrum of a rare earth-based broad spectrum passive cooling fiber fabric.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the inventive concepts pertain. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The reflective rare earth compound prepared by mixing and calcining the rare earth phosphate, the titanium dioxide and the alumina has high reflectivity within the range of 300-2500 nm, and can reflect the heat of sunlight by more than 85%; the rare earth composite silicate combines with excellent emissivity quality of various elements, the far infrared emissivity of the rare earth composite silicate is more than 0.95 at 8-13 mu m, and the efficient passive refrigeration can be realized; the rare earth silicate has lower heat conductivity and heat insulation, and the materials act together to show excellent passive cooling and heat insulation effects. Furthermore, the hollow structure gives it excellent heat insulating properties in hot environments (fig. 1). The nano rare earth particles are successfully prepared, and are directly mixed with the polymer base material to prepare the spinning master batch, so that the preparation is convenient and the cost is low.
The invention will be described in detail with reference to examples.
Example 1 (preparation of reflective rare earth complexes)
(1) Preparing rare earth phosphate:
uniformly dispersing anhydrous lanthanum carbonate into water at 85 ℃, adding phosphoric acid under stirring until no bubbles are generated in the solution, adjusting the pH to 7 by ammonia water, and carrying out suction filtration and drying at 100 ℃ to obtain lanthanum phosphate (the XRD spectrum of lanthanum phosphate is shown in figure 2).
The method is adopted to prepare cerium phosphate, yttrium phosphate, gadolinium phosphate, samarium phosphate, ytterbium phosphate, europium phosphate, holmium phosphate, erbium phosphate, lanthanum cerium phosphate and yttrium cerium phosphate respectively.
(2) Preparing a reflective rare earth compound:
the prepared lanthanum phosphate, titanium dioxide and aluminum oxide are mixed according to the following proportion of 1:1: the mass ratio of 1 is uniformly mixed by a solid-phase high-speed mixer, and calcined at 1200 ℃ for 4 hours to obtain the reflective rare earth compound (the XRD spectrum of the reflective rare earth compound is shown in figure 3).
The prepared cerium phosphate, titanium dioxide and aluminum oxide are prepared according to the following weight ratio of 1:0.5: the reflective rare earth compound is prepared by adopting the method according to the mass ratio of 1.
The yttrium phosphate, titanium dioxide and alumina prepared are mixed according to the following ratio of 1:0.6: the reflective rare earth compound is prepared by adopting the method according to the mass ratio of 0.9.
The prepared samarium phosphate, titanium dioxide and aluminum oxide are mixed according to the following ratio of 1:0.7: the reflective rare earth compound is prepared by adopting the method according to the mass ratio of 0.8.
Ytterbium phosphate, titanium pigment and alumina prepared according to the following ratio of 1:0.8: the reflective rare earth compound is prepared by adopting the method according to the mass ratio of 0.7.
The europium phosphate, titanium dioxide and alumina prepared are mixed according to the following ratio of 1:0.9: the reflective rare earth compound is prepared by adopting the method according to the mass ratio of 0.6.
The prepared holmium phosphate, titanium dioxide and aluminum oxide are prepared according to the following weight ratio of 1:1.2: the reflective rare earth compound is prepared by adopting the method according to the mass ratio of 0.5.
The prepared erbium phosphate, titanium dioxide and alumina are mixed according to the following ratio of 1:1.5: the reflective rare earth compound is prepared by adopting the method according to the mass ratio of 0.4.
The prepared lanthanum cerium phosphate, titanium dioxide and aluminum oxide are prepared according to the following weight ratio of 1:1.7: the reflective rare earth compound is prepared by adopting the method according to the mass ratio of 0.2.
The prepared yttrium cerium phosphate, titanium dioxide and aluminum oxide are prepared according to the following weight ratio of 1:2: the reflective rare earth compound is prepared by adopting the method according to the mass ratio of 0.1.
Example 2 (rare earth composite silicate)
Lanthanum carbonate, yttrium carbonate and silicon oxide are mixed according to a mole ratio of 1:1: placing 1 into a ball mill, adding deionized water to make the solid content be 60%, ball-milling 12 h at a rotation speed of 200 r/min, taking out, suction-filtering and drying, calcining 4 h at 1500 ℃, taking out, continuously ball-milling 12 h, suction-filtering and drying to obtain yttrium lanthanum silicate (figure 4 is XRD spectrum of yttrium lanthanum silicate).
Lanthanum carbonate, cerium carbonate and silicon oxide are prepared into lanthanum cerium silicate according to the method.
Cerium carbonate, yttrium carbonate and silicon oxide are prepared into yttrium cerium silicate according to the method.
Lanthanum silicate is prepared by the method of lanthanum carbonate, zirconium carbonate and silicon oxide.
Yttrium silicate is prepared by the method of yttrium carbonate, zirconium carbonate and silicon oxide.
Lanthanum carbonate, gadolinium carbonate and silicon oxide are prepared into lanthanum gadolinium silicate according to the method.
Example 3 (preparation of polyester fiber and fiber Material)
The rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber comprises the following components in parts by weight: lanthanum phosphate, titanium dioxide and alumina 1:1:1, 5.5 parts of reflective rare earth compound obtained by calcination, 4.5 parts of yttrium lanthanum silicate, 2 parts of silane coupling agent, 2 parts of antioxidant and 86 parts of polyethylene terephthalate.
The preparation method of the rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber comprises the following steps:
pre-dispersing the reflective rare earth compound obtained in the example 1, the yttrium lanthanum silicate obtained in the example 2 and the silane coupling agent in deionized water, uniformly mixing, shearing and dispersing for 2 hours at a linear speed of 9 m/s by a sand mill to obtain rare earth passive cooling nano slurry, wherein the particle size distribution D in the slurry 90 About 500 nm.
Concentrating the rare earth passive cooling nano slurry by a reduced pressure distillation mode, and uniformly mixing the polyethylene terephthalate, the concentrated slurry and the antioxidant by a high-speed mixer. And (3) drying at 100-130 ℃, carrying out melt extrusion granulation at 290 ℃ and a granulating speed of 200 r/min and 30 m/min, wherein the water content is lower than 200 ppm, and obtaining the rare earth-based broad spectrum cooling heat insulation master batch. And drying the master batch, and preparing the rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber by using an annular hollow spinneret plate through a melt spinning process after the water content is lower than 200 ppm, wherein the spinning temperature is 300 ℃, and the winding speed is 4000 m/min.
The rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric is obtained by knitting the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric in a knitting mode. The reflectivity spectrum diagram of the rare earth-based broad-spectrum passive cooling heat-insulating fiber fabric is shown in figure 5.
Example 4 (preparation of nylon fiber and fiber Shell fabric)
The rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber comprises the following components in parts by weight: lanthanum phosphate, titanium dioxide and alumina 1:1:1, 0.55 part of reflective rare earth compound obtained by calcination, 0.45 part of lanthanum yttrium silicate, 2 parts of silane coupling agent, 2 parts of antioxidant and 95 parts of polyamide 6 powder.
The preparation method of the rare earth-based broad spectrum passive cooling hollow heat insulation nylon fiber is the same as that of the embodiment 3. The rare earth-based broad spectrum passive cooling hollow heat insulation nylon fiber of the embodiment is knitted in a knitting mode to obtain the rare earth-based broad spectrum passive cooling heat insulation fiber nylon fabric.
Example 5
The rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber comprises the following components in parts by weight: samarium phosphate, titanium white and alumina 1:1:1, 0.05 part of reflective rare earth compound obtained by calcination, 0.05 part of yttrium cerium silicate, 2.9 parts of silane coupling agent, 2 parts of antioxidant and 95 parts of polyethylene powder.
The preparation method of the rare earth-based broad spectrum passive cooling hollow heat insulation nylon fiber is the same as that of the embodiment 3. The rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric is obtained by knitting the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric in a knitting mode.
Example 6
The rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber comprises the following components in parts by weight: europium phosphate, titanium dioxide and alumina 1:1:1, 2.8 parts of reflective rare earth compound obtained by calcination, 1.2 parts of zirconium yttrium silicate, 0.1 part of silane coupling agent, 0.9 part of antioxidant and 95 parts of polyurethane powder.
The preparation method of the rare earth-based broad spectrum passive cooling hollow heat insulation nylon fiber is the same as that of the embodiment 3. The rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric is obtained by knitting the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric in a knitting mode.
Example 7
The rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber comprises the following components in parts by weight: cerium lanthanum phosphate, titanium dioxide and alumina 1:1:1, 4.2 parts of reflective rare earth compound obtained by calcination, 2.8 parts of lanthanum gadolinium silicate, 2 parts of silane coupling agent, 1 part of antioxidant and 90 parts of polyurethane powder.
The preparation method of the rare earth-based broad spectrum passive cooling hollow heat insulation nylon fiber is the same as that of the embodiment 3. The rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric is obtained by knitting the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric in a knitting mode.
Comparative example 1 (reflective rare earth composite without titanium white added)
The rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber comprises the following components in parts by weight: lanthanum phosphate and alumina 1:1, 5.5 parts of reflective rare earth compound obtained by calcination, 4.5 parts of yttrium lanthanum silicate, 2 parts of silane coupling agent, 2 parts of antioxidant and 86 parts of polyethylene terephthalate.
The preparation method of the rare earth-based broad-spectrum passive cooling hollow heat-insulating polyester fiber is the same as that of the embodiment 3. The rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric is obtained by knitting the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric in a knitting mode.
Comparative example 2 (no alumina added to the reflective rare earth composite)
The rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber comprises the following components in parts by weight: lanthanum phosphate and titanium dioxide 1:1, 5.5 parts of reflective rare earth compound obtained by calcination, 4.5 parts of yttrium lanthanum silicate, 2 parts of silane coupling agent, 2 parts of antioxidant and 86 parts of polyethylene terephthalate.
The preparation method of the rare earth-based broad-spectrum passive cooling hollow heat-insulating polyester fiber is the same as that of the embodiment 3. The rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric is obtained by knitting the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric in a knitting mode.
Comparative example 3 (no rare earth phosphate added to reflective rare earth composite)
The rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber comprises the following components in parts by weight: alumina and titanium dioxide 1:1, 5.5 parts of reflective rare earth compound obtained by calcination, 4.5 parts of yttrium lanthanum silicate, 2 parts of silane coupling agent, 2 parts of antioxidant and 86 parts of polyethylene terephthalate.
The preparation method of the rare earth-based broad-spectrum passive cooling hollow heat-insulating polyester fiber is the same as that of the embodiment 3. The rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric is obtained by knitting the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber fabric in a knitting mode.
Comparative example 4 (without addition of reflective rare earth composite)
The heat insulation fiber C comprises the following components in parts by weight: 10 parts of yttrium lanthanum silicate, 2 parts of a silane coupling agent, 2 parts of an antioxidant and 86 parts of polyethylene terephthalate.
The preparation method comprises the following steps: will be solidThe lanthanum yttrium silicate and the silane coupling agent obtained in example 2 are pre-dispersed in deionized water, and after being uniformly mixed, the mixture is sheared and dispersed for 2 hours at a high speed by a sand mill at a linear speed of 9 m/s, so as to obtain the cooling nano slurry, wherein the particle size distribution D in the slurry is obtained 90 About 500 nm.
The preparation method of the heat-insulating fiber is the same as in example 3. The heat-insulating fiber of the comparative example was knitted by knitting to obtain a heat-insulating fiber fabric.
Comparative example 5 (reflective rare earth composite not calcined)
The heat-insulating fiber comprises the following components in parts by weight: 1.5 parts of lanthanum phosphate, 1.5 parts of titanium dioxide, 1.5 parts of aluminum oxide, 4.5 parts of yttrium lanthanum silicate, 2 parts of a silane coupling agent, 2 parts of an antioxidant and 86 parts of polyethylene terephthalate. Wherein lanthanum yttrium silicate is the lanthanum yttrium silicate prepared in example 2.
The preparation method comprises the following steps: pre-dispersing lanthanum phosphate, titanium dioxide, aluminum oxide, yttrium lanthanum silicate and a silane coupling agent in deionized water, uniformly mixing, shearing and dispersing for 2 hours at a linear speed of 9 m/s by a sand mill to obtain a cooling nano slurry, wherein the particle size distribution D in the slurry is obtained 90 About 500 nm.
The preparation method of the heat-insulating fiber is the same as in example 3. The heat-insulating fiber of the comparative example was knitted by knitting to obtain a heat-insulating fiber fabric.
Comparative example 6 (no rare earth complex silicate added)
The heat insulation fiber E comprises the following components in parts by weight: lanthanum phosphate, titanium dioxide and alumina 1:1:1, 10 parts of a reflective rare earth compound obtained by calcination, 2 parts of a silane coupling agent, 2 parts of an antioxidant and 86 parts of polyethylene terephthalate.
The preparation method comprises the following steps: pre-dispersing the reflective rare earth compound obtained in the example 1 and the silane coupling agent in deionized water, uniformly mixing, shearing and dispersing for 2 hours at a high speed by a sand mill at a linear speed of 9 m/s to obtain a cooling nano slurry, wherein the particle size distribution D in the slurry 90 About 500 nm.
The preparation method of the heat-insulating fiber is the same as in example 3. The heat-insulating fiber E of this comparative example was knitted by knitting to obtain a heat-insulating fiber fabric.
Comparative example 7 (Single rare earth silicate)
The heat insulation fiber F comprises the following components in parts by weight: lanthanum phosphate, titanium dioxide and alumina 1:1:1, 5.5 parts of a reflective rare earth compound obtained by calcination, 4.5 parts of lanthanum silicate, 2 parts of a silane coupling agent, 2 parts of an antioxidant and 86 parts of polyethylene terephthalate.
The preparation method comprises the following steps: pre-dispersing the reflective rare earth compound obtained in the example 1, lanthanum silicate and silane coupling agent in deionized water, uniformly mixing, shearing and dispersing for 2 hours at a linear speed of 9 m/s by a sand mill to obtain a cooling nano slurry, wherein the particle size distribution D in the slurry is obtained 90 About 500 nm.
The preparation method of the heat-insulating fiber is the same as in example 3. The heat-insulating fiber of this comparative example was knitted by knitting to obtain a heat-insulating fiber fabric F.
Comparative example 8 (fiber shape is a generally circular fiber)
The passive cooling fiber comprises the following components in parts by weight: lanthanum phosphate, titanium dioxide and alumina 1:1:1, 5.5 parts of reflective rare earth compound obtained by calcination, 4.5 parts of yttrium lanthanum silicate, 2 parts of silane coupling agent, 2 parts of antioxidant and 86 parts of polyethylene terephthalate.
The preparation method of the passive cooling fiber was the same as in example 3, except that the annular hollow spinneret was replaced with a common spinneret. The passive cooling fiber of the comparative example is woven in a knitting mode to obtain the passive cooling fiber fabric.
Comparative example 9 (blank)
Directly granulating, melt spinning and knitting the polyethylene terephthalate powder to obtain the fabric.
The fabrics obtained in example 3 and comparative examples 1 to 9 were tested for reflectance in the 300-2500 nm band and far infrared emissivity in the 8-13 μm band, and the temperature difference at the fabric cover after 30 minutes of irradiation of the solar light simulation lamp was tested with reference to comparative example 9 (blank), and the results are shown in the following table:
table 1 results of fabric performance tests of examples and comparative examples
Comparative example 9 is a blank cloth sample, no functional component is added, and the thermal insulation performance of the fabric is better as the temperature rise of the comparative fabric and the experimental fabric is larger. The results of the table show that after the rare earth passive cooling powder is added, the visible-near infrared reflection and far infrared emission properties of the fabric are improved, and the fabric has good heat insulation and cooling properties.
Specifically, the comparative data of comparative examples 1-3 and example 3 shows that the rare earth phosphate in the reflective rare earth compound and the alumina of the titanium pigment have a synergistic effect, and when no titanium pigment is added, the reflectance of the visible wave band is reduced to 300-2500 nm; when alumina is not added, the reflecting layer is not compact enough, and the reflectivity is low; the reduced near infrared band reflection results in a lower total solar reflectance of 300-2500 nm without the addition of rare earth phosphate.
A comparison of comparative example 4 and example 3 shows that the solar reflectance and emissivity of the swatches are greatly reduced without the addition of the reflective rare earth compound.
A comparison of comparative example 5 and example 3 shows that the mixed calcination of lanthanum phosphate, titanium dioxide and alumina helps to reduce defects in the system and improve the reflective properties of the material.
The comparison of comparative example 6, comparative example 7 and example 3 shows that the addition of rare earth composite silicate can improve the emissivity of the fabric to more than 0.94, and the emission effect is poor without adding rare earth composite silicate or single silicate. In addition, when rare earth silicate is not added, the heat preservation property of the fabric is poor, and the heat insulation effect is also reduced to a certain extent.
Comparison of comparative example 8 and example 3 shows that, when the hollow structure of the fiber is changed to a general solid structure, the heat insulation performance of the fabric is further lowered than comparative example 6 and comparative example 7, and the heat insulation effect is further lowered, although the reflection and emission properties of the fabric are higher.
Comparative example 10 (slurry particle size distribution was too large)
Lanthanum phosphate, titanium dioxide and alumina 1:1:1, 18 parts of reflective rare earth compound obtained by calcination, 22 parts of lanthanum yttrium silicate and 8 parts of silane coupling agent are uniformly mixed in 52 parts of deionized water, and ball-milling is carried out for 3 h by a ball mill at the rotating speed of 200 r/min, thus obtaining passive cooling slurry with the particle size distribution D in the slurry 90 About 5 μm.
The passive cooling slurry of the comparative example was mixed with polyester powder, and after drying, the master batch had been hollow and wrinkled during the granulation process, and the spinning process could not be performed due to excessive pressure.
This comparative example shows that controlling the particle size distribution of the slurry is critical to the smooth performance of the spinning process, while maintaining the material properties, to reduce the particle size of the functional component as much as possible.
Comparative example 11 (preparation of rare earth phosphate)
Dispersing lanthanum carbonate into water at 60 ℃, adding phosphoric acid under stirring until no bubbles are generated in the solution, adjusting the pH to 7 by ammonia water, enabling the solution to be very viscous, difficult to suction-filter, and calcining at 1000 ℃ for more than 4 hours during suction-filtering to obtain lanthanum phosphate.
The comparative example shows that when the reaction temperature is lower than 80 ℃, the reaction solution becomes sticky, which causes difficult post-treatment and increases the process cost, so that the temperature of the system in the experimental process should be controlled to be 80-100 ℃.
Comparative example 12 (preparation of rare earth silicate)
Placing yttrium carbonate and silicon oxide into a ball mill, adding deionized water to ensure that the solid content is 60%, ball milling at the rotating speed of 200 r/min for 12 h, taking out, filtering, drying, calcining at 1500 ℃ for 4 h, and taking out to obtain yttrium silicate, wherein the caking is serious and the XRD spectrum has more miscellaneous peaks.
This comparative example shows that the ball milling step after calcination helps to obtain a high purity product and reduces the difficulty of post-treatment.
The above embodiments are merely preferred embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A rare earth-based broad spectrum passive cooling hollow heat insulation fiber is characterized in that: comprises the following components in percentage by weight:
0.1% -10% of rare earth passive cooling powder;
85% -95% of base material powder;
1% -10% of an auxiliary agent;
wherein, the rare earth passive cooling powder comprises the following components in percentage by weight: 50-70% of reflective rare earth compound and 30-50% of rare earth compound silicate;
the reflective rare earth compound is obtained by calcining rare earth phosphate, titanium dioxide and aluminum oxide together; the rare earth composite silicate comprises one or more than two of lanthanum cerium silicate, lanthanum yttrium silicate, yttrium cerium silicate, zirconium lanthanum silicate, zirconium yttrium silicate and lanthanum gadolinium silicate.
2. The rare earth-based broad spectrum passive cooling hollow heat insulating fiber according to claim 1, wherein: the mass ratio of the rare earth phosphate, the titanium dioxide and the alumina in the reflective rare earth compound is 1: (0.5-2): (0.1-1).
3. The rare earth-based broad spectrum passive cooling hollow heat insulating fiber according to claim 1, wherein: the rare earth phosphate comprises one or more of lanthanum phosphate, cerium phosphate, yttrium phosphate, gadolinium phosphate, samarium phosphate, ytterbium phosphate, europium phosphate, holmium phosphate, erbium phosphate, lanthanum cerium phosphate and yttrium cerium phosphate.
4. The rare earth-based broad spectrum passive cooling hollow heat insulating fiber according to claim 1, wherein: the base material powder is one or more of polyethylene, polypropylene, polyethylene terephthalate, polylactic acid, polyacrylonitrile, polyamide, ethylene-octene copolymer, polybutylene terephthalate, polypropylene terephthalate, polyurethane and polyvinyl alcohol.
5. The rare earth-based broad spectrum passive cooling hollow heat insulating fiber according to claim 1, wherein: the auxiliary agent is one or more of dispersing agent, antioxidant, slipping agent and release agent.
6. The rare earth-based broad spectrum passive cooling hollow heat insulating fiber according to claim 1, wherein: the preparation method of the reflective rare earth compound comprises the following steps:
(1) Uniformly dispersing 4N-level rare earth carbonate into deionized water at 80-100 ℃ with the concentration of 50-500 g/L, slowly dropwise adding phosphoric acid into the deionized water under mechanical stirring at the rotation speed of 200 r/min-1000 r/min until no bubbles are generated in the solution, adding a pH regulator to adjust the pH to be neutral, carrying out suction filtration and drying, and obtaining rare earth phosphate at the drying temperature of 90-110 ℃;
(2) And (3) uniformly mixing the rare earth phosphate obtained in the step (1) with titanium pigment and aluminum oxide by a solid-phase high-speed mixer, and placing the mixture into a muffle furnace for calcination at 900-1600 ℃ to obtain the reflective rare earth compound.
7. The rare earth-based broad spectrum passive cooling hollow heat insulating fiber according to claim 1, wherein: the preparation method of the rare earth composite silicate comprises the following steps:
uniformly dispersing the first carbonate, the second carbonate and the silicon oxide in deionized water, wherein the solid content is 30% -80%, placing the obtained dispersion in a ball mill, ball-milling for 12-24 hours at a rotating speed of 200-500 r/min, carrying out suction filtration and drying, wherein the drying temperature is 90-110 ℃, calcining in a muffle furnace, taking out, carrying out secondary ball milling at a rotating speed of 200-500 r/min, wherein the ball-milling solid content is 30% -80%, the ball-milling time is 12-24 hours, and carrying out suction filtration and drying, and the drying temperature is 90-110 ℃, thus obtaining the rare earth composite silicate;
the first carbonate and the second carbonate are different and are respectively and independently selected from one of lanthanum carbonate, cerium carbonate, zirconium carbonate, yttrium carbonate and gadolinium carbonate.
8. The rare earth-based broad spectrum passive cooling hollow heat insulating fiber according to claim 7, wherein: the mole ratio of the first carbonate to the second carbonate to the silicon oxide is 1:1:1.
9. the method for preparing the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber according to any one of claims 1 to 8, which is characterized in that: the method comprises the following steps:
(1) Pre-dispersing the reflective rare earth compound, rare earth compound silicate and auxiliary agent in deionized water, uniformly mixing, shearing and dispersing at a high speed for 0.5-10 h by a sand mill, wherein the shearing line speed is 5 m/s-13 m/s, obtaining rare earth passive cooling nano slurry with the particle size distribution of 100-800 nm, concentrating the nano slurry by removing water through reduced pressure distillation, dispersing base material powder into concentrated slurry, adding the auxiliary agent, and uniformly mixing by a high-speed mixer to obtain a mixture;
(2) Drying the mixture obtained in the step (1) at 100-130 ℃, carrying out melt extrusion granulation at a melting temperature of 150-350 ℃ and an extrusion speed of 100-300 r/min and a granulating speed of 10-30 m/min, and obtaining rare earth-based broad spectrum cooling heat insulation master batch;
(3) And (3) drying the rare earth-based broad spectrum cooling heat-insulating master batch obtained in the step (2), and preparing the rare earth-based broad spectrum passive cooling hollow heat-insulating fiber by using an annular hollow spinneret plate through a melt spinning process after the water content is lower than 200 ppm, wherein the spinning temperature is 150-350 ℃, and the winding speed is 1800-5000 m/min.
10. Use of the rare earth-based broad spectrum passive cooling hollow thermal insulation fiber according to any one of claims 1-8 in the field of clothing fabrics, home textiles, industrial textiles and outdoor fabric products.
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