CN117468119A - Rare earth phosphate composite salt passive cooling function administration fiber and preparation method thereof - Google Patents
Rare earth phosphate composite salt passive cooling function administration fiber and preparation method thereof Download PDFInfo
- Publication number
- CN117468119A CN117468119A CN202311798644.5A CN202311798644A CN117468119A CN 117468119 A CN117468119 A CN 117468119A CN 202311798644 A CN202311798644 A CN 202311798644A CN 117468119 A CN117468119 A CN 117468119A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- composite salt
- fiber
- passive cooling
- preparing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 91
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 86
- 150000003839 salts Chemical class 0.000 title claims abstract description 71
- 239000002131 composite material Substances 0.000 title claims abstract description 68
- -1 Rare earth phosphate Chemical class 0.000 title claims abstract description 47
- 238000001816 cooling Methods 0.000 title claims abstract description 47
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 42
- 239000010452 phosphate Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000004744 fabric Substances 0.000 claims abstract description 46
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 84
- 150000002910 rare earth metals Chemical class 0.000 claims description 43
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 34
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 23
- 229910021641 deionized water Inorganic materials 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 18
- 239000002861 polymer material Substances 0.000 claims description 18
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 17
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 17
- 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 15
- 239000002270 dispersing agent Substances 0.000 claims description 14
- 229910000164 yttrium(III) phosphate Inorganic materials 0.000 claims description 14
- UXBZSSBXGPYSIL-UHFFFAOYSA-K yttrium(iii) phosphate Chemical compound [Y+3].[O-]P([O-])([O-])=O UXBZSSBXGPYSIL-UHFFFAOYSA-K 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 13
- 238000001125 extrusion Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000002074 melt spinning Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- 238000009987 spinning Methods 0.000 claims description 9
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 8
- 239000004698 Polyethylene Substances 0.000 claims description 7
- 239000001993 wax Substances 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 239000012188 paraffin wax Substances 0.000 claims description 5
- 238000004804 winding Methods 0.000 claims description 5
- 150000002009 diols Chemical class 0.000 claims description 4
- 235000019359 magnesium stearate Nutrition 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- JXSRRBVHLUJJFC-UHFFFAOYSA-N 7-amino-2-methylsulfanyl-[1,2,4]triazolo[1,5-a]pyrimidine-6-carbonitrile Chemical compound N1=CC(C#N)=C(N)N2N=C(SC)N=C21 JXSRRBVHLUJJFC-UHFFFAOYSA-N 0.000 claims description 2
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 2
- GWOWVOYJLHSRJJ-UHFFFAOYSA-L cadmium stearate Chemical compound [Cd+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O GWOWVOYJLHSRJJ-UHFFFAOYSA-L 0.000 claims description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
- 235000013539 calcium stearate Nutrition 0.000 claims description 2
- 239000008116 calcium stearate Substances 0.000 claims description 2
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000009413 insulation Methods 0.000 abstract description 6
- 230000005855 radiation Effects 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 3
- 238000005057 refrigeration Methods 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000009941 weaving Methods 0.000 description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 description 8
- 238000009940 knitting Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 229920000642 polymer Polymers 0.000 description 4
- 230000004075 alteration Effects 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000004595 color masterbatch Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000036559 skin health Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QQCIBICIISNSAY-UHFFFAOYSA-K terbium(3+);phosphate Chemical compound [Tb+3].[O-]P([O-])([O-])=O QQCIBICIISNSAY-UHFFFAOYSA-K 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a fiber for taking rare earth phosphate composite salt with a passive cooling function and a preparation method thereof, wherein the step 1 is to prepare the rare earth phosphate composite salt; step 2, preparing functional fiber master batches; and 3, preparing the passive cooling functional fiber. The fabric prepared by the rare earth phosphate composite salt passive cooling function clothing fiber has strong sunlight reflection capability and radiation refrigeration capability, and meanwhile, the fiber fabric has good processing and preparation properties, has better air permeability and comfort compared with a coating type heat insulation fabric, and can not generate the conditions of coating falling off and heat insulation property attenuation after washing after long-time use.
Description
Technical Field
The invention belongs to the field of textile weaving, and particularly relates to a rare earth phosphate composite salt passive cooling function clothing fiber and a preparation method thereof.
Background
It is well known that the outdoor temperature is high in sunny summer, and great discomfort is brought to the user. Moreover, high-intensity direct sunlight can cause a certain degree of burn to the skin even if the sunlight irradiates for a long time, and great hidden trouble is brought to the skin health of human bodies. Therefore, the demand for light, thin, comfortable, breathable and heat-insulating fabrics is becoming more urgent.
Disclosure of Invention
In view of the above, the invention aims to overcome the defects in the prior art and provides a fiber for passive cooling function of rare earth phosphate composite salt and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
a preparation method of rare earth phosphate composite salt passive cooling function administration fiber comprises the following steps:
step 1 is to prepare rare earth phosphoric acid composite salt:
dispersing lanthanum cerium phosphate, yttrium phosphate and cerium oxide into deionized water, dropwise adding phosphoric acid into the deionized water under the condition of stirring, regulating pH to be neutral after the reaction is completed, and carrying out suction filtration, drying and calcination on the obtained mixed solution to obtain the rare earth phosphoric acid composite salt;
step 2, preparing functional fiber master batch:
mixing the rare earth phosphate composite salt with a dispersing agent, drying, and then carrying out melt extrusion granulation with a first part of dried polymer material to obtain the functional fiber master batch;
step 3, preparing passive cooling functional fiber:
and (3) carrying out batch mixing and drying on the functional fiber master batch and the second part of polymer material, and preparing the passive cooling functional fiber through a melt spinning process.
Further, the molar ratio of lanthanum cerium phosphate, yttrium phosphate and cerium oxide in the step 1 is 1:0.1-10:0.1-10; the ratio of the sum of the mass of the lanthanum cerium phosphate, the mass of the yttrium phosphate and the mass of the cerium oxide in the step 1 to the volume of deionized water is 50-500 g/L; the temperature of the deionized water in the step 1 is 80-100 ℃.
The rare earth phosphate is doped with elements with different radiuses such as lanthanum, cerium, yttrium and the like, so that lattice distortion occurs to the rare earth phosphate, the reflection band range of the material is enlarged, and the emission performance of the material is improved. Meanwhile, the color of the functional master batch can be adjusted by adjusting the proportion of white yttrium phosphate, green lanthanum cerium phosphate and yellow cerium oxide.
Under the high-temperature processing condition, the cerium oxide is extremely easy to accelerate the degradation of the polymer melt, so that the mechanical properties of the fiber are poor, and therefore, the rare earth phosphate composite salt is coated by adding the dispersing agent, so that the dispersibility of the rare earth phosphate composite salt in the melt is improved, and meanwhile, the damage to the chemical bonds of the polymer is reduced.
Further, the particle size of the rare earth phosphate composite salt in the step 1 is 80-150nm; the speed of the dripping step in the step 1 is less than or equal to 2 ml/min; the rotating speed of the stirring step in the step 1 is 200-1000 r/min; the temperature of the drying step in the step 1 is 90-110 ℃; the temperature of the calcining step in the step 1 is 900-1200 ℃.
The speed of adding phosphoric acid dropwise is controlled within 2 ml/min, the calcining temperature is 900-1200 ℃, the prepared rare earth functional material is ensured to be nano-scale while the specific crystal form rare earth phosphoric acid composite salt is obtained, and the nano-scale rare earth phosphoric acid composite salt can be directly dispersed into polymer powder for granulating and spinning.
Further, the dispersing agent in the step 2 is at least one of polyethylene wax, polyamide wax, paraffin wax, zinc stearate, barium stearate, calcium stearate, cadmium stearate, magnesium stearate, copper stearate, acetylenic diol or ethylene bis-stearamide; the addition amount of the dispersing agent is 0.5-1% of the mass of the functional fiber master batch.
Further, the temperature of the drying step of the rare earth phosphate composite salt in the step 2 is 110-130 ℃ and the time is 8-12h; the water content of the rare earth phosphoric acid composite salt in the step 2 after being dried is lower than 30ppm; the temperature of the drying step of the first part of high polymer materials in the step 2 is 60-130 ℃ and the time is 8-16h; and (2) the water content of the first part of high polymer materials in the step (2) after being dried is lower than 200ppm.
Further, the mass ratio of the rare earth phosphate composite salt in the step 2 to the first part of high polymer material is 0.1-30:70-99.9; the melting temperature of the melting extrusion step in the step 2 is 150-350 ℃, the bracing water temperature is 60-80 ℃, the extrusion speed is 100-300r/min, and the granulating speed is 30-70m/min.
Further, the mass ratio of the functional fiber master batch to the second part of high polymer material in the step 3 is 5-30:70-100; the temperature of the drying step in the step 3 is 60-130 ℃, the time is 8-16h, and the water content of the materials after the drying step is finished is lower than 200ppm; the spinning temperature of the melt spinning process in the step 3 is 150-350 ℃, and the winding speed is 1800-5000m/min.
Further, the first part of polymer material is one of PE, PP, PET, PLA, PAN, PA, POE, PBT, PTT or TPU; the second part of high polymer material is one of PE, PP, PET, PLA, PAN, PA, POE, PBT, PTT and TPU.
The invention also provides a fiber for passive cooling function of rare earth phosphate composite salt prepared by the preparation method, wherein the fiber is prepared from functional fiber master batch by a melt spinning process; the functional fiber master batch comprises 1-30wt% of rare earth functional material and 70-99wt% of polymer material.
The invention also provides application of the rare earth phosphate composite salt passive cooling function clothing fiber in preparing fabrics, fabrics or ready-made clothes.
Compared with the prior art, the invention has the following advantages:
the fabric prepared by the rare earth phosphate composite salt passive cooling function clothing fiber has strong sunlight reflection capability and radiation refrigeration capability, and meanwhile, the fiber fabric has good processing and preparation properties, has better air permeability and comfort compared with a coating type heat insulation fabric, and can not generate the conditions of coating falling off and heat insulation property attenuation after washing after long-time use. In addition, the fabric prepared by utilizing the colors of the rare earth elements has the advantages of bright colors, permanent color fastness and the like, removes the dyeing link of the fabric, reduces the discharge of dyeing wastewater, and has certain environmental protection advantages.
The rare earth phosphate composite salt passive cooling functional administration fiber prepares a passive cooling rare earth functional material by selecting, compounding and blending the rare earth phosphate composite salt and a dispersing agent, the functional material has good reflection capability on visible-near infrared light with the wavelength of 400-2500 nm, reduces the absorption of solar radiation energy, has good infrared emission and transmission capability on an atmospheric window of 8-13 mu m, promotes the heat exchange of human body heat with the universe environment in a heat radiation mode, and realizes zero energy consumption cooling through radiation refrigeration; the fiber adjusts the ratio of lanthanum cerium phosphate to cerium oxide in the rare earth functional material, and prepares the color shade of the prepared master batch, so that the color of the final fiber and the fabric product can be regulated and controlled, and the purpose of dyeing-free is achieved. Under the condition of combining multiple functions, the fabric prepared from the master batch has the function of passively cooling, can effectively reduce the surface temperature of a human body by 3-9 ℃, and has a more comfortable cool feeling effect.
The passive cooling functional fiber disclosed by the invention can be prepared by proportioning and blending all components according to different application scene requirements, and the functional fiber color master batch can be added in proportion in the fiber preparation process, so that dyeing-free fibers and fabrics with the passive cooling function are obtained. Compared with the heat-insulating fabric in the prior art, the heat-insulating fabric has the advantages of high efficiency in isolating external heat, quick heat conduction and dissipation in human body, comfortable wearing in contact with cool feeling, no dyeing, environmental protection, no pollution emission, water washing resistance and the like.
Drawings
Fig. 1 is a cross-sectional view of a functional fiber master batch according to example 1 of the present invention.
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 present invention pertains. 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 present invention will be described in detail with reference to examples.
Example 1
A preparation method of rare earth phosphate composite salt passive cooling function administration fiber comprises the following steps:
step 1 is to prepare rare earth phosphoric acid composite salt:
dispersing lanthanum cerium phosphate, yttrium phosphate and cerium oxide in a mass ratio of 1:1:9 into deionized water at 80 ℃, slowly dropwise adding phosphoric acid into the deionized water at a speed of less than 2 ml/min under the stirring condition of a rotating speed of 500 r/min, adding ammonia water to adjust the pH value to be neutral after the reaction is finished, and carrying out suction filtration, drying at 100 ℃ and calcining at 1200 ℃ on the obtained mixed solution to obtain the rare earth phosphoric acid composite salt (yellow);
step 2, preparing functional fiber master batch:
mixing 29.5 parts of rare earth phosphate composite salt with 0.5 part of dispersing agent (paraffin, zinc stearate and acetylenic diol with the mass ratio of 4:4:2), drying for 12 hours at 120 ℃, and then carrying out melt extrusion granulation on the mixture with 70 parts of PET (with the water content of 30 ppm) after drying (dynamic drying for 4 hours at 80 ℃ and drying for 8 hours after heating to 110 ℃), wherein the PET is put into a main feeding bin, the mixture of the rare earth phosphate composite salt and the dispersing agent is put into a side feeding bin, metering and feeding are carried out according to the proportion of 7/3 of the feeding mass ratio of main feeding to side feeding, and melt extrusion is carried out at 260 ℃ to obtain functional fiber master batch, and the cross section is shown in figure 1;
step 3, preparing passive cooling functional fiber:
mixing 30 parts of functional fiber master batch and 70 parts of PET uniformly by a rotary drum, and preparing rare earth passive cooling pre-oriented fiber (POY) by melt spinning of a single screw extruder, wherein the spinning temperature is 275 ℃, the winding speed is 2800m/min, the fiber fineness is 120D, and the elongation at break is 120%. The environment temperature is 25 ℃ and the humidity is 60% in the spinning process, and the assembly pressure is not higher than 18Mpa. And (3) placing the prepared POY fiber for balancing for 48 hours, and then stretching and false twisting (DTY process) to obtain the rare earth passive cooling stretch textured yarn with the specification of 75D/48 f.
And (3) weaving test: the DTY fiber is used for preparing the functional fabric with plain stitch through a weft knitting process, the temperature difference between the inside and outside of the fabric is 8.1 ℃ under the irradiation of sunlight, and no obvious chromatic aberration exists after the fabric is washed for 50 times.
Example 2
A preparation method of rare earth phosphate composite salt passive cooling function administration fiber comprises the following steps:
step 1 is to prepare rare earth phosphoric acid composite salt:
dispersing lanthanum cerium phosphate, yttrium phosphate and cerium oxide with the mass ratio of 1:9:1 into deionized water at 80 ℃, slowly dropwise adding phosphoric acid into the deionized water at the concentration of 200g/L under the stirring condition with the rotating speed of 500 r/min at the speed of less than 2 ml/min until no bubbles are generated in the solution, adding ammonia water to adjust the pH value to be neutral after the reaction is finished, carrying out suction filtration on the obtained mixed solution, drying at 100 ℃, and calcining at 1200 ℃ to obtain the rare earth phosphoric acid composite salt (white);
step 2, preparing functional fiber master batch:
mixing 24 parts of rare earth phosphate composite salt with 1 part of dispersing agent (paraffin wax, zinc stearate, magnesium stearate and polyamide wax with the mass ratio of 3:3:2:2), drying for 12 hours at 120 ℃, carrying out melt extrusion granulation on the mixture and 75 parts of PA6 (with the water content of 157 ppm) subjected to dynamic drying for 12 hours at 120 ℃, putting the PA6 into a main feeding bin, putting the mixture of the rare earth phosphate composite salt and the dispersing agent into a side feeding bin, metering and feeding the mixture according to the feeding mass ratio of 3/1 of the main feeding/side feeding, and carrying out melt extrusion at 270 ℃ to obtain functional fiber master batch;
step 3, preparing passive cooling functional fiber:
mixing 30 parts of functional fiber master batch and 70 parts of PA6 uniformly by a rotary drum, and preparing rare earth passive cooling pre-oriented fiber (POY) by melt spinning by a single screw extruder, wherein the spinning temperature is 280 ℃, the drafting multiple is 3.5 times, the winding speed is 2200m/min, the fiber fineness is 200D, and the breaking elongation is 30%. The environment temperature is 25 ℃ and the humidity is 60% in the spinning process, and the assembly pressure is not higher than 15Mpa. Obtaining the rare earth passive cooling function fully-drawn textured yarn with the specification of 200D/72 f.
And (3) weaving test: the DTY fiber is used for preparing the functional fabric with plain stitch through a weft knitting process, the temperature difference between the inside and outside of the fabric under the irradiation of sunlight is 6.6 ℃, and no obvious color difference exists after the fabric is washed for 50 times.
Example 3
A preparation method of rare earth phosphate composite salt passive cooling function administration fiber comprises the following steps:
step 1 is to prepare rare earth phosphoric acid composite salt:
dispersing lanthanum cerium phosphate, yttrium phosphate and cerium oxide in a mass ratio of 9:1:1 into deionized water at 80 ℃, slowly dropwise adding phosphoric acid into the deionized water at a speed of less than 2 ml/min under the stirring condition of a rotating speed of 500 r/min, adding ammonia water to adjust the pH value to be neutral after the reaction is finished, and carrying out suction filtration, drying at 100 ℃ and calcining at 1200 ℃ on the obtained mixed solution to obtain the rare earth phosphoric acid composite salt (green);
step 2, preparing functional fiber master batch:
mixing 24.5 parts of rare earth phosphate composite salt with 0.5 part of dispersing agent (polyethylene wax, paraffin wax, magnesium stearate and acetylenic diol with the mass ratio of 3:3:2:2), drying for 12 hours at 120 ℃, enabling the water content to be 28ppm, then carrying out melt extrusion granulation with 75 parts of PLA (water content to be 80 ppm) after drying (dynamic drying for 4 hours at 80 ℃ and drying for 8 hours after heating to 120 ℃), putting PLA into a main feeding bin, putting the mixture of the rare earth phosphate composite salt and the dispersing agent into a side feeding bin, metering and feeding according to the ratio of 3/1 of the feeding mass ratio of main feeding to side feeding, and carrying out melt extrusion at 265 ℃ to obtain functional fiber master batch;
step 3, preparing passive cooling functional fiber:
taking 20 parts of functional fiber master batches and 80 parts of PLA, uniformly mixing the functional fiber master batches and the PLA through a rotary drum, and preparing the rare earth passive cooling pre-oriented fiber (POY) through melt spinning of a single screw extruder, wherein the spinning temperature is 270 ℃, the winding speed is 2800m/min, the fiber fineness is 80D, and the elongation at break is 120%. The environment temperature is 25 ℃ and the humidity is 60% in the spinning process, and the assembly pressure is not higher than 16Mpa. And (3) placing the prepared POY fiber for balancing for 48 hours, and then stretching and false twisting (DTY process) to obtain the rare earth passive cooling function stretch textured yarn with the specification of 50D/36 f.
And (3) weaving test: the DTY fiber is used for preparing the functional fabric with plain stitch through a weft knitting process, the temperature difference between the inside and outside of the fabric is 6.8 ℃ under the irradiation of sunlight, and no obvious chromatic aberration exists after the fabric is washed for 50 times.
Comparative example 1
The preparation method of the rare earth phosphate composite salt passive cooling function administration fiber is different from the embodiment 1 only in that:
step 1 is to prepare rare earth phosphoric acid composite salt:
dispersing lanthanum cerium phosphate and yttrium phosphate with the mass ratio of 1:1 into deionized water at 80 ℃ and the concentration of 200g/L, slowly dripping phosphoric acid into the deionized water at the speed of less than 2 ml/min under the stirring condition with the rotating speed of 500 r/min, adding ammonia water to adjust the pH value to be neutral after the reaction is finished, and carrying out suction filtration, drying at 100 ℃ and calcining at 1200 ℃ on the obtained mixed solution to obtain the rare earth phosphoric acid composite salt.
And (3) weaving test: the DTY fiber is used for preparing the functional fabric with plain stitch through a weft knitting process, the temperature difference between the inside and outside of the fabric is 4.5 ℃ under the irradiation of sunlight, and no obvious chromatic aberration exists after 50 times of washing.
Comparative example 2
Step 1 is to prepare rare earth phosphoric acid composite salt:
dispersing yttrium phosphate and cerium oxide with the mass ratio of 1:9 into deionized water at 80 ℃ and the concentration of 200g/L, slowly dripping phosphoric acid into the deionized water at the speed of less than 2 ml/min under the stirring condition of the rotating speed of 500 r/min, adding ammonia water to adjust the pH value to be neutral after the reaction is finished, and carrying out suction filtration, drying at 100 ℃ and calcining at 1200 ℃ on the obtained mixed solution to obtain the rare earth phosphoric acid composite salt.
And (3) weaving test: the DTY fiber is used for preparing the functional fabric with plain stitch through a weft knitting process, the temperature difference between the inside and outside of the fabric is 4.3 ℃ under the irradiation of sunlight, and no obvious color difference exists after the fabric is washed for 50 times.
Comparative example 3
Step 1 is to prepare rare earth phosphoric acid composite salt:
dispersing lanthanum cerium phosphate and cerium oxide with the mass ratio of 1:9 into deionized water with the temperature of 80 ℃ and the concentration of 200g/L, slowly dripping phosphoric acid into the deionized water at the speed of less than 2 ml/min under the stirring condition with the rotating speed of 500 r/min, adding ammonia water to adjust the pH value to be neutral after the reaction is finished, and carrying out suction filtration, drying at the temperature of 100 ℃ and calcining at the temperature of 1200 ℃ on the obtained mixed solution to obtain the rare earth phosphoric acid composite salt.
And (3) weaving test: the DTY fiber is used for preparing the functional fabric with plain stitch through a weft knitting process, the temperature difference between the inside and outside of the fabric under the irradiation of sunlight is 3.9 ℃, and no obvious color difference exists after the fabric is washed for 50 times.
Comparative example 4
The preparation method of the rare earth phosphate composite salt passive cooling function administration fiber is different from the embodiment 1 only in that:
step 1 is to prepare rare earth phosphoric acid composite salt:
dispersing lanthanum cerium phosphate, terbium phosphate and cerium oxide in a mass ratio of 1:1:9 into deionized water at 80 ℃ to obtain a concentration of 200g/L, slowly dropwise adding phosphoric acid into the mixture at a speed of less than 2 ml/min under the stirring condition with a rotating speed of 500 r/min, adding ammonia water to adjust the pH value to be neutral after the reaction is finished, and carrying out suction filtration, drying at 100 ℃ and calcining at 1200 ℃ on the obtained mixed solution to obtain the rare earth phosphoric acid composite salt.
And (3) weaving test: the DTY fiber is used for preparing the functional fabric with plain stitch through a weft knitting process, the temperature difference between the inside and outside of the fabric is 4.3 ℃ under the irradiation of sunlight, and no obvious color difference exists after the fabric is washed for 50 times.
Comparative example 5
The preparation method of the rare earth phosphate composite salt passive cooling function administration fiber is different from the embodiment 1 only in that:
step 1 is to prepare rare earth phosphoric acid composite salt:
dispersing europium cerium phosphate, yttrium phosphate and cerium oxide with the mass ratio of 1:1:9 into deionized water at 80 ℃, slowly dropwise adding phosphoric acid into the deionized water at the speed of 500 r/min at the speed of less than 2 ml/min, adding ammonia water to adjust the pH value to be neutral after the reaction is finished, and carrying out suction filtration, drying at 100 ℃ and calcining at 1200 ℃ on the obtained mixed solution to obtain the rare earth phosphoric acid composite salt.
And (3) weaving test: the obtained DTY fiber is used for preparing the functional fabric with plain stitch through a weft knitting process, the temperature difference between the inside and outside of the fabric under the irradiation of sunlight is 4.2 ℃, and no obvious color difference exists after the fabric is washed for 50 times.
Comparative example 6
And (3) carrying out melt spinning on the PET polymer slice through a single screw extruder to prepare fibers, weaving the fibers into fabrics, and testing the temperature difference between the inside and the outside of the fabrics under the irradiation of sunlight at 2.5 ℃.
The products obtained in each example and comparative example were examined, and the results are shown in Table 1.
TABLE 1 detection results
As shown in Table 1, compared with example 1, comparative examples 1-3 changed the composition of the rare earth phosphate complex salt, the far infrared emission and emission performance of the fabric were greatly reduced, and the heat insulation properties of the fabric were greatly affected. The addition of yttrium phosphate can enhance reflectivity, and lanthanum cerium phosphate and cerium oxide can enhance far infrared emissivity. Comparative examples 4 to 5 have smaller radii of other rare earth compound ions and are not stable enough in doping structure as compared with example 1. The covalent radiuses of lanthanum, cerium and yttrium ions are closest, lattice doping is easier to carry out, the emission and reflection properties of the material are improved, and the fabric shows good heat insulation performance. In comparative example 6, the rare earth phosphate complex salt is not added at all, the infrared emissivity and the emissivity are greatly reduced, and the passive cooling function is lost.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. A preparation method of rare earth phosphate composite salt passive cooling function administration fiber is characterized by comprising the following steps: the method comprises the following steps:
step 1 is to prepare rare earth phosphoric acid composite salt:
dispersing lanthanum cerium phosphate, yttrium phosphate and cerium oxide into deionized water, dropwise adding phosphoric acid into the deionized water under the condition of stirring, regulating pH to be neutral after the reaction is completed, and carrying out suction filtration, drying and calcination on the obtained mixed solution to obtain the rare earth phosphoric acid composite salt;
step 2, preparing functional fiber master batch:
mixing the rare earth phosphate composite salt with a dispersing agent, drying, and then carrying out melt extrusion granulation with a first part of dried polymer material to obtain the functional fiber master batch;
step 3, preparing passive cooling functional fiber:
and (3) carrying out batch mixing and drying on the functional fiber master batch and the second part of polymer material, and preparing the passive cooling functional fiber through a melt spinning process.
2. The method for preparing the rare earth phosphoric acid composite salt passive cooling function administration fiber according to claim 1, which is characterized in that: the molar ratio of the lanthanum cerium phosphate to the yttrium phosphate to the cerium oxide in the step 1 is 1:0.1-10:0.1-10; the ratio of the sum of the mass of the lanthanum cerium phosphate, the mass of the yttrium phosphate and the mass of the cerium oxide in the step 1 to the volume of deionized water is 50-500 g/L; the temperature of the deionized water in the step 1 is 80-100 ℃.
3. The method for preparing the rare earth phosphoric acid composite salt passive cooling function administration fiber according to claim 1, which is characterized in that: the particle size of the rare earth phosphate composite salt in the step 1 is 80-150nm; the speed of the dripping step in the step 1 is less than or equal to 2 ml/min; the rotating speed of the stirring step in the step 1 is 200-1000 r/min; the temperature of the drying step in the step 1 is 90-110 ℃; the temperature of the calcining step in the step 1 is 900-1200 ℃.
4. The method for preparing the rare earth phosphoric acid composite salt passive cooling function administration fiber according to claim 1, which is characterized in that: the dispersing agent in the step 2 is at least one of polyethylene wax, polyamide wax, paraffin wax, zinc stearate, barium stearate, calcium stearate, cadmium stearate, magnesium stearate, copper stearate, acetylenic diol or ethylene bis stearamide; the addition amount of the dispersing agent is 0.5-1% of the mass of the functional fiber master batch.
5. The method for preparing the rare earth phosphoric acid composite salt passive cooling function administration fiber according to claim 1, which is characterized in that: the temperature of the drying step of the rare earth phosphate composite salt in the step 2 is 110-130 ℃ and the time is 8-12h; the water content of the rare earth phosphoric acid composite salt in the step 2 after being dried is lower than 30ppm; the temperature of the drying step of the first part of high polymer materials in the step 2 is 60-130 ℃ and the time is 8-16h; and (2) the water content of the first part of high polymer materials in the step (2) after being dried is lower than 200ppm.
6. The method for preparing the rare earth phosphoric acid composite salt passive cooling function administration fiber according to claim 1, which is characterized in that: the mass ratio of the rare earth phosphate composite salt in the step 2 to the first part of high polymer material is 0.1-30:70-99.9; the melting temperature of the melting extrusion step in the step 2 is 150-350 ℃, the bracing water temperature is 60-80 ℃, the extrusion speed is 100-300r/min, and the granulating speed is 30-70m/min.
7. The method for preparing the rare earth phosphoric acid composite salt passive cooling function administration fiber according to claim 1, which is characterized in that: the mass ratio of the functional fiber master batch to the second part of high polymer material in the step 3 is 5-30:70-100; the temperature of the drying step in the step 3 is 60-130 ℃, the time is 8-16h, and the water content of the materials after the drying step is finished is lower than 200ppm; the spinning temperature of the melt spinning process in the step 3 is 150-350 ℃, and the winding speed is 1800-5000m/min.
8. The method for preparing the rare earth phosphoric acid composite salt passive cooling function administration fiber according to claim 1, which is characterized in that: the first part of polymer material is one of PE, PP, PET, PLA, PAN, PA, POE, PBT, PTT or TPU; the second part of high polymer material is one of PE, PP, PET, PLA, PAN, PA, POE, PBT, PTT and TPU.
9. A fiber for passive cooling function of rare earth phosphate composite salt prepared by the preparation method of claim 1, which is characterized in that: the fiber is prepared from functional fiber master batches through a melt spinning process; the functional fiber master batch comprises 1-30wt% of rare earth functional material and 70-99wt% of polymer material.
10. The use of the rare earth phosphate complex salt passive cooling function administration fiber as claimed in claim 9, characterized in that: the fiber is applied to preparing fabrics, fabrics or ready-made clothes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311798644.5A CN117468119B (en) | 2023-12-26 | 2023-12-26 | Rare earth phosphate composite salt passive cooling function administration fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311798644.5A CN117468119B (en) | 2023-12-26 | 2023-12-26 | Rare earth phosphate composite salt passive cooling function administration fiber and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN117468119A true CN117468119A (en) | 2024-01-30 |
| CN117468119B CN117468119B (en) | 2024-02-27 |
Family
ID=89629660
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311798644.5A Active CN117468119B (en) | 2023-12-26 | 2023-12-26 | Rare earth phosphate composite salt passive cooling function administration fiber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117468119B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303814A (en) * | 1999-12-16 | 2001-07-18 | 化成光学仪器株式会社 | Rare earth phosphate and its preparing process and rare earth phosphate phosphor |
| CN102530904A (en) * | 2011-12-17 | 2012-07-04 | 赣州虔东稀土集团股份有限公司 | Preparation method of crystalline high-purity rare earth phosphate with controllable granularity |
| CN102585572A (en) * | 2012-02-29 | 2012-07-18 | 上海师范大学 | Heat-reflecting heat-insulation inorganic composite material as well preparation method and application thereof |
| CN102849706A (en) * | 2012-08-29 | 2013-01-02 | 深圳大学 | Preparation method of cerium phosphate nano-wires |
| CN114525676A (en) * | 2022-04-25 | 2022-05-24 | 天津包钢稀土研究院有限责任公司 | Rare earth-based infrared reflection thermal fabric and preparation method and application thereof |
| CN116239301A (en) * | 2023-03-07 | 2023-06-09 | 上海太洋科技有限公司 | Phosphate optical glass and preparation method thereof |
| CN116715883A (en) * | 2023-05-16 | 2023-09-08 | 武汉理工大学 | Rare earth reinforced composite film with low-temperature high-efficiency radiation heat dissipation function and preparation method thereof |
-
2023
- 2023-12-26 CN CN202311798644.5A patent/CN117468119B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303814A (en) * | 1999-12-16 | 2001-07-18 | 化成光学仪器株式会社 | Rare earth phosphate and its preparing process and rare earth phosphate phosphor |
| CN102530904A (en) * | 2011-12-17 | 2012-07-04 | 赣州虔东稀土集团股份有限公司 | Preparation method of crystalline high-purity rare earth phosphate with controllable granularity |
| CN102585572A (en) * | 2012-02-29 | 2012-07-18 | 上海师范大学 | Heat-reflecting heat-insulation inorganic composite material as well preparation method and application thereof |
| CN102849706A (en) * | 2012-08-29 | 2013-01-02 | 深圳大学 | Preparation method of cerium phosphate nano-wires |
| CN114525676A (en) * | 2022-04-25 | 2022-05-24 | 天津包钢稀土研究院有限责任公司 | Rare earth-based infrared reflection thermal fabric and preparation method and application thereof |
| CN116239301A (en) * | 2023-03-07 | 2023-06-09 | 上海太洋科技有限公司 | Phosphate optical glass and preparation method thereof |
| CN116715883A (en) * | 2023-05-16 | 2023-09-08 | 武汉理工大学 | Rare earth reinforced composite film with low-temperature high-efficiency radiation heat dissipation function and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN117468119B (en) | 2024-02-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101255614B (en) | Inorganic solid-phase combination powder, master batch and manufacture method, fibre and manufacture method | |
| CN107190382B (en) | A kind of polyester blended fabric and preparation method thereof that graphene is modified | |
| CN106149091A (en) | A kind of preparation method of the antibacterial coloured environment-friendly polyester fiber of high fire-retardance | |
| CN102174719A (en) | Microporous photocatalyst bamboo charcoal polyester modified short fiber and preparation method thereof | |
| CN106367844A (en) | Sheath core fiber with night light far infrared function and preparation method thereof | |
| CN114539773B (en) | Long-acting antibacterial high-temperature-resistant stock solution coloring master batch and preparation method and application thereof | |
| CN102443876A (en) | Preparation method for polyester fiber with compound ultraviolet ray resisting, aging resisting, moisture absorbing and quick drying functions | |
| CN117468119B (en) | Rare earth phosphate composite salt passive cooling function administration fiber and preparation method thereof | |
| CN115161802A (en) | Preparation method of antibacterial and anti-ultraviolet sheath-core regenerated polyester fiber | |
| CN103882548A (en) | Functional nylon 66 fiber and preparation method thereof | |
| CN117385492B (en) | Hollow cooling fiber modified by lanthanum and cerium natural distribution product and preparation method thereof | |
| CN102877154B (en) | Method for preparing organic pigment microcapsule polyester color yarn | |
| CN111560167B (en) | Preparation method of anti-ultraviolet polyamide color master batch and functional fiber | |
| CN104047069A (en) | Photochromic fiber making method | |
| CN101545170B (en) | Method for weaving olefine environmentally-friendly cloth | |
| TWI418676B (en) | Fibers having infrared absorption ability, fabrication methods thereof and fabrics containing the same | |
| CN104342777B (en) | A kind of polyester monofilament with far-infrared functional and preparation method thereof | |
| CN116024683A (en) | Light-absorbing, heating and heat-accumulating antibacterial viscose fiber and preparation method thereof | |
| CN117468120B (en) | Rare earth-based cooling heat insulation special-shaped fiber and preparation method thereof | |
| CN101314870B (en) | Method for preparing fibre | |
| CN109056099B (en) | Production process of super-soft high-elasticity colored silk fiber | |
| CN111809271A (en) | High-performance nano ceramic uvioresistant high-thermal insulation fiber and preparation method thereof | |
| CN117385485B (en) | Rare earth-based broad-spectrum passive cooling hollow heat-insulating fiber and preparation method and application thereof | |
| CN115717281B (en) | Antibacterial composite polyester fiber and preparation method thereof | |
| CN116949595A (en) | Ultraviolet-proof yarn and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |