CN108842217A - It is a kind of with magnetism, far infrared, antibacterial functions composite fibre - Google Patents

It is a kind of with magnetism, far infrared, antibacterial functions composite fibre Download PDF

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Publication number
CN108842217A
CN108842217A CN201810591916.7A CN201810591916A CN108842217A CN 108842217 A CN108842217 A CN 108842217A CN 201810591916 A CN201810591916 A CN 201810591916A CN 108842217 A CN108842217 A CN 108842217A
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Prior art keywords
filler
polyester
nano particle
hollow
nano
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Inventor
罗鼎明
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Foshan Nanhai Beauty Underwear Co Ltd
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Foshan Nanhai Beauty Underwear Co Ltd
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Priority to CN201810591916.7A priority Critical patent/CN108842217A/en
Publication of CN108842217A publication Critical patent/CN108842217A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent 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
    • D01F6/92Monocomponent 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/12Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
    • C08G63/16Dicarboxylic acids and dihydroxy compounds
    • C08G63/18Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
    • C08G63/181Acids containing aromatic rings
    • C08G63/183Terephthalic acids
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Artificial Filaments (AREA)

Abstract

This application involves it is a kind of with magnetism, far infrared, antibacterial functions composite fibre, which is a kind of polyester complex fiber, and the polyester complex fiber is using polyester as substrate, using filler A, filler B and filler C as additive, blended is prepared by melting;It is characterized in that, wherein, filler A includes:ZrO2Nano-powder and dispersing agent;Filler B includes:Tourmaline nano particle and dispersing agent;Filler C includes:Nano silver grain and dispersing agent.

Description

It is a kind of with magnetism, far infrared, antibacterial functions composite fibre
Technical field
This application involves composite fibre field more particularly to it is a kind of with magnetism, far infrared, antibacterial functions compound fibre Dimension.
Background technique
Far infrared is beneficial to human body, and electromagnetic wave of the wavelength in 0.76~1000 μm of region is called infrared ray, by 2.5~ The infrared ray of 1000 μ m wavelength ranges becomes far infrared, and far infrared has following feature:Radiance, RESONANCE ABSORPTION and Permeability.Currently, the functionalization exploitation of textile is more and more important with the development of industrialization technology;By in fiber or spinning Addition has the substance of far infrared transmission property in fabric, can absorb the heat that solar energy and human body distribute, and be transmitted back to The far infrared that needed by human body is wanted plays positive warming effect using thermogenetic effect of the far infrared to human body, meanwhile, have Promote blood circulation of human body and metabolism, has the function of eliminating fatigue, regain one's strength.
In the prior art, usually the powder with far-infrared transmitting function is added in fabric, has it certain Far-infrared transmitting function, however, in the prior art, the far infrared transmissivity of generally existing room temperature far infrared powder is relatively low etc. is asked Topic.
Existing simple function fiber is used for function textile, can only directionally solve the problems, such as one aspect.With The continuous improvement of living standards of the people and the raising of industry, health care, military industry field textile application standard, multi-functional spinning Fabric is the new trend of textile future development, and this kind of product has wide in fields such as civilian, industry, health care, military projects The market space.
Preparing multifunctional composite fiber, there are two types of approach:First is that the fiber of selection different function carries out plying processing, it is made Multifunctional yarn, however its effect is to be improved;Second is that directly raw by multiple groups part compined spinning apparatus and spinning technique technology Produce function and service fiber type.
Summary of the invention
The present invention is intended to provide it is a kind of with magnetism, far infrared, antibacterial functions composite fibre, to solve set forth above ask Topic.
Provided in the embodiment of the present invention it is a kind of with magnetism, far infrared, antibacterial functions composite fibre, the compound fibre Dimension is a kind of polyester complex fiber, and the polyester complex fiber is using polyester as substrate, using filler A, filler B and filler C as additive, By melting blended be prepared;It is characterized in that, wherein, filler A includes:ZrO2Nano-powder and dispersing agent;Filler B Including:Tourmaline nano particle and dispersing agent;Filler C includes:Nano silver grain and dispersing agent.
The technical solution that the embodiment of the present invention provides can include the following benefits:
1, the compound fibre of polyester is prepared by the way that melting is blended using filler A, filler B and filler C as additive in the present invention Dimension, by control mass ratio, above-mentioned filler A, filler B and filler C synergistic effect so that the polyester functional fibre be provided with it is negative Ion, magnetism, far infrared transmission and antibacterial functions have expanded the application range of polyester fiber significantly;
It 2, include dispersing agent in the filler A, filler B and filler C, due to special pattern, the dispersing agent is poly- It can effectively prevent the reunion of additive in ester fiber preparation process, be conducive to the performance of above-mentioned function, achieve unexpected Beneficial effect.
The additional aspect of the application and advantage will be set forth in part in the description, and will partially become from the following description It obtains obviously, or recognized by the practice of the application.It should be understood that above general description and following detailed description are only Be it is exemplary and explanatory, the application can not be limited.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawings, but the embodiment in attached drawing is not constituted to any limit of the invention System, for those of ordinary skill in the art, without creative efforts, can also obtain according to the following drawings Other attached drawings.
Fig. 1 is the composed structure schematic diagram of composite fibre of the present invention;
1- filler A, 2- filler B, 3- filler C, 4- polyester.
Specific embodiment
Example embodiments are described in detail here, and the example is illustrated in the accompanying drawings.Following description is related to When attached drawing, unless otherwise indicated, the same numbers in different drawings indicate the same or similar elements.Following exemplary embodiment Described in embodiment do not represent all embodiments consistented with the present invention.On the contrary, they be only with it is such as appended The example of device and method being described in detail in claims, some aspects of the invention are consistent.
Embodiments herein be related to it is a kind of with magnetism, far infrared, antibacterial functions composite fibre, which is A kind of polyester complex fiber, specifically, the polyester complex fiber is addition with filler A, filler B and filler C using polyester as substrate Agent, by melting blended be prepared;In terms of content, raw material includes according to weight percent:16% filler A, 4% Filler B, 3% filler C, surplus are polyester.
Wherein, filler A is the nanocomposite with far infrared transmission performance;Filler B is to send out with anion Penetrate the nanocomposite of performance;Filler C is the nanocomposite with anti-microbial property.
In order to reach technical effect, filler A includes:ZrO2Nano-powder and dispersing agent;Filler B includes:Tourmaline Nano particle and dispersing agent;Filler C includes:Nano silver grain and dispersing agent.
In order to enable polyester fiber has anion and infrared emission performance, in the prior art, usually in polyester fiber Addition has the powder of anion or far infrared transmission performance in preparation process, so that polyester fiber has anion or infrared Emitting performance;For example, in the prior art, having and being melted by the way that tourmaline powder, sepiolite, pearl powder to be added in polyester fondant Melt spinning, polyester fiber with health care function is made;However, those skilled in the art understand that, usual nano material Partial size is smaller, and surface-active and free energy are higher, causes the nano particle of addition to have agglomeration tendency, this will largely effect on function Energy property particle plays a role;Meanwhile causing polyester fiber modified effect unobvious.
In technical solution of the present invention, using filler A, filler B and filler C as additive, by melt it is blended be prepared it is poly- Ester composite fibre, by controlling mass ratio, above-mentioned filler A, filler B and filler C synergistic effect, so that the polyester functional fibre Anion, magnetism, far infrared transmission and antibacterial functions are provided with, have expanded the application range of polyester fiber significantly;In addition, described Filler A, filler B and filler C in include dispersing agent, due to special pattern, the dispersing agent is in polyester fiber preparation process In can effectively prevent the reunion of additive, be conducive to the performance of above-mentioned function, achieve unexpected beneficial effect.
In order to realize the technical solution of the application, which preferably uses hollow Fe3O4Nano particle, as a result, this implementation In mode, filler A includes:ZrO2Nano-powder and hollow Fe3O4Nano particle, filler B include tourmaline nano particle and Hollow Fe3O4Nano particle, filler C include Nano silver grain and hollow Fe3O4Nano particle.
Also, the hollow Fe3O4Nano particle is prepared by solvent-thermal method.
Specifically, the hollow Fe3O4Nano particle diameter is 250nm.
Ferrous oxide and ferroso-ferric oxide are all the oxides of iron, wherein ferroso-ferric oxide is usually expressed as band and is magnetic Black crystals, with good electric conductivity, and oxidisability and reproducibility and deposit, be widely used in magnetic material, biology Medical material and heavy metal ion adsorbed field.Since it is with excellent physicochemical properties, using more and more extensive, so And in the prior art, it is few to be used in polyester fiber as functional filler, in technical solution of the present invention, by molten A kind of Fe of hollow structure is prepared in agent thermal method3O4Nano particle, and by its creative dispersing agent as filler, by this Dispersing agent with the powder mixed calcining with anion, far infrared transmission and antibacterial functions, utilizes hollow Fe respectively3O4Nanometer The magnetism of grain, can by it with anion, far infrared, antimicrobial nano particle be respectively in connection with effectively preventing anion, far infrared With the reunion of antimicrobial powder in the polyester, unexpected technical effect is produced.
It is far infrared additive about filler A, filler A, wherein the ZrO2Nano-powder is to pass through ultrasonic microemulsion liquid Method preparation.
Currently, the exploitation about far-infrared material is concentrated mainly on far-infrared ceramic powder, far-infrared ceramic powder master If containing Mn, Fe, Co and its oxide, however, currently, the average particle size of room temperature far-infrared ceramic powder still in micron order, Its far infrared radiation rate is relatively low.ZrO2Powder is production zirconium oxide special cermacis, high grade refractory, optical communication device, new energy The basic material of source material, ZrO2With low-temperature sintering, ZrO2Nano-powder is as a kind of non-toxic and non-radioactive and has low The material of warm far infrared transmission performance is a kind of important far infrared additive;However, if by above-mentioned ZrO2Nano-powder is straight It connects and is added in polyester fiber, due to nanometer reuniting effect, ZrO2Nano-powder disperses unevenly in polyester fiber, can significantly Reduce the performance of far infrared performance;In technical scheme, by by ZrO2Nano-powder and hollow Fe3O4Nano particle point Powder mixing, calcining, have obtained filler A, have then been added into polyester fiber again.In above-mentioned mixing, calcination process, so that ZrO2Nano-powder can be adsorbed effectively and be incorporated in hollow Fe3O4Nano grain surface substantially increases far infrared transmission Uniformity produces unexpected technical effect.
Preferably, in filler A, the mass fraction of each substance is:ZrO215 parts of nano-powder, hollow Fe3O4Nano particle 4 Part;The ZrO2The partial size of nano-powder is 20nm.
It is anionic additive about filler B, filler B, wherein the tourmaline nano particle diameter is 100nm.
Tourmaline is a kind of natural electrode with similar to magnet poles, and tourmaline is widely used in environmental protection, day The often numerous areas such as life, for example, tourmaline powder is added in artificial silk, since tourmaline powder has positive and negative electrode, After human contact, countless weak currents can be generated in skin surface, stimulate blood circulation, form negative ion effect;However, In this field, tourmaline is directly used in textile, electronegative ion can not be played well.Technical solution of the present invention In, by by tourmaline nano particle and hollow Fe3O4Nanoparticie dispersion agents mixing, calcining, have obtained filler B, then again will It is added in polyester fiber.In above-mentioned mixing, calcination process, due to hollow Fe3O4Nano particle and tourmaline nano particle are equal Certain magnetism is showed, which can be such that the two effectively combines, and substantially increase the uniformity of anion emission, produce meaning Technical effect unexpectedly.
Preferably, in filler B, the mass fraction of each substance is:17 parts of tourmaline nano particle, hollow Fe3O4Nano particle 11 parts.
It is antibacterial additives about filler C, filler C, wherein the Nano silver grain partial size is 50nm.
Preferably, in filler C, the mass fraction of each substance is:10 parts of Nano silver grain, hollow Fe3O47 parts of nano particle.
Further explanation is made to the present invention below with reference to embodiment.
Embodiment 1
It is a kind of with magnetism, far infrared, antibacterial functions composite fibre, the composite fibre be a kind of polyester complex fiber, Specifically, the polyester complex fiber using polyester as substrate, using filler A, filler B and filler C as additive, passes through the blended system of melting It is standby to obtain;In terms of content, raw material includes according to weight percent:16% filler A, 4% filler B, 3% filler C, Surplus is polyester.
It wherein, is far infrared additive about filler A, filler A, filler A includes:ZrO2Nano-powder and hollow Fe3O4It receives The mass fraction of rice grain, each substance is:ZrO215 parts of nano-powder, hollow Fe3O44 parts of nano particle;The ZrO2Nano-powder Partial size be 20nm, the hollow Fe3O4Nano particle diameter is 250nm;
It wherein, is anionic additive about filler B, filler B, filler B includes:Tourmaline nano particle and hollow Fe3O4The mass fraction of nano particle, each substance is:17 parts of tourmaline nano particle, hollow Fe3O411 parts of nano particle;It is described Tourmaline nano particle diameter be 100nm, the hollow Fe3O4Nano particle diameter is 250nm;
It wherein, is antibacterial additives about filler C, filler C, filler C includes:Nano silver grain and hollow Fe3O4Nanometer The mass fraction of particle, each substance is:10 parts of Nano silver grain, hollow Fe3O47 parts of nano particle;The nano grain of silver seed Diameter is 50nm, the hollow Fe3O4Nano particle diameter is 250nm.
It the following is the preparation process of the polyester complex fiber:
Step 1, dispersing agent is prepared
Weigh FeCl3·6H2O, hexamethylenetetramine, polyvinylpyrrolidone are respectively 1.35g, 0.28g, 0.7g, will be upper It states substance to be successively dissolved in ethylene glycol, forms mixed solution, wherein ethylene glycol volume is 30ml, then magnetic agitation, after stirring The mixed solution is transferred in ptfe autoclave, reaction kettle is put into electric drying oven with forced convection, is protected at 220 DEG C Warm 15h after the reaction was completed takes out reaction kettle, cooled to room temperature, and the powder that reaction obtains is centrifuged, then It is cleaned by ultrasonic with distilled water, powder is then obtained into hollow Fe after 75 DEG C of dry 9h in a vacuum drying oven3O4Nano particle;
Step 2 prepares zirconium oxide presoma
By the ZrOCl of 720g/L2·8H2The ethylenediamine tetra-acetic acid of O and 94g/L is according to volume ratio 2:1 mixing, is vigorously stirred 30min make its be uniformly mixed, obtain transparent micro emulsion, then with ammonium hydroxide adjust pH value be 11.4, the ultrasound 14min at 84 DEG C, Ultrasonic power is 20KHz, obtains clear gel, is then washed with distilled water to AgNO3Solution inspection does not measure Cl-, then use Ethanol washing 3 times, the zirconium oxide presoma after washing is put into thermostatic drying chamber, in 60 DEG C of dry 15h;
Step 3 prepares filler A, filler B and filler C
By zirconium oxide presoma, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, and are sufficiently stirred It mixes uniformly, obtains far infrared additive slurry A, be then baked to, under nitrogen protection in 500 DEG C of calcining 3h, pulverize, Up to filler A;
By tourmaline nano particle, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, sufficiently It stirs evenly, obtains anionic additive slurry B, be then baked to, under nitrogen protection in 410 DEG C of calcining 3h, be ground into Powder is to get filler B;
By Nano silver grain, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, and are sufficiently stirred Uniformly, obtain antibacterial additives slurry C, be then baked to, under nitrogen protection in 300 DEG C of calcining 3h, pulverize to get Filler C;
Step 4 prepares polyester master particle
Firstly, filler A, filler B, filler C and ethylene glycol are mixed, ultrasound 5h at room temperature after stirring obtains mixed liquor; Then mixed liquor and p-phthalic acid, catalyst aid are esterified, polymerize, obtains polyester master particle;
Wherein, esterification temperature is 260 DEG C, pressure 280kPa, and polycondensation reaction is carried out when esterification yield reaches greater than 96.5%, is contracted Poly- temperature is 290 DEG C, is evacuated to 20MPa, when polycondensation to inherent viscosity is 0.74 deciliter/gram, discharging, and blank;
Step 5 prepares polyester preoriented yarn
Polyester master particle is melted, filter is then fed into and is filtered, after metering, into spinning pack, then will be sprayed Tow carry out it is cooling, oil, preoriented yarn is wound into after deflector roll, wherein spinning temperature is 285 DEG C, and spinning speed is 3400m/min;
Step 6 prepares polyester complex fiber
Polyester preoriented yarn can be prepared into polyester functional fibre after a roller, hot tank, two rollers, scroll tube, winding, wherein Draft speed is 500m/min, and draw ratio 3.1, a roll temperature is 90 DEG C, and two roll temperatures are 140 DEG C.
The far-infrared radiated property of fiber is characterized by measuring the normal emittance of polyester complex fiber in the present embodiment, Inspection result shows that its normal emittance is 0.96, and quasi- about the assessment of bids of far infrared performance according to this field, normal emittance is greater than Far-infrared textiles can be assessed as equal to 0.8, the polyester complex fiber in the present embodiment is met the requirements of the standard;
Measure the anionic property of polyester complex fiber in the present embodiment:
It is detected using air ion concentration relative standard's measuring device, the polyester fiber that the application is obtained and common Polyester fiber is cut into 10 × 10cm respectively2Size, apart from above-mentioned detection device 6.5cm2Air inlet 2mm or so, measure air Middle negative ion concentration, the polyester fiber anion emission number for obtaining the application is 4126 anion/cm3, and conventional polyester The negative ion concentration of fiber is substantially zeroed, illustrates that the polyester fiber of the application has good anion emission performance.
Embodiment 2
It is a kind of with magnetism, far infrared, antibacterial functions composite fibre, the composite fibre be a kind of polyester complex fiber, Specifically, the polyester complex fiber using polyester as substrate, using filler A, filler B and filler C as additive, passes through the blended system of melting It is standby to obtain;In terms of content, raw material includes according to weight percent:16% filler A, 10% filler B, 3% filler C, surplus is polyester.
It wherein, is far infrared additive about filler A, filler A, filler A includes:ZrO2Nano-powder and hollow Fe3O4It receives The mass fraction of rice grain, each substance is:ZrO215 parts of nano-powder, hollow Fe3O44 parts of nano particle;The ZrO2Nano-powder Partial size be 20nm, the hollow Fe3O4Nano particle diameter is 250nm;
It wherein, is anionic additive about filler B, filler B, filler B includes:Tourmaline nano particle and hollow Fe3O4The mass fraction of nano particle, each substance is:17 parts of tourmaline nano particle, hollow Fe3O411 parts of nano particle;It is described Tourmaline nano particle diameter be 100nm, the hollow Fe3O4Nano particle diameter is 250nm;
It wherein, is antibacterial additives about filler C, filler C, filler C includes:Nano silver grain and hollow Fe3O4Nanometer The mass fraction of particle, each substance is:10 parts of Nano silver grain, hollow Fe3O47 parts of nano particle;The nano grain of silver seed Diameter is 50nm, the hollow Fe3O4Nano particle diameter is 250nm.
It the following is the preparation process of the polyester complex fiber:
Step 1, dispersing agent is prepared
Weigh FeCl3·6H2O, hexamethylenetetramine, polyvinylpyrrolidone are respectively 1.35g, 0.28g, 0.7g, will be upper It states substance to be successively dissolved in ethylene glycol, forms mixed solution, wherein ethylene glycol volume is 30ml, then magnetic agitation, after stirring The mixed solution is transferred in ptfe autoclave, reaction kettle is put into electric drying oven with forced convection, is protected at 220 DEG C Warm 15h after the reaction was completed takes out reaction kettle, cooled to room temperature, and the powder that reaction obtains is centrifuged, then It is cleaned by ultrasonic with distilled water, powder is then obtained into hollow Fe after 75 DEG C of dry 9h in a vacuum drying oven3O4Nano particle;
Step 2 prepares zirconium oxide presoma
By the ZrOCl of 720g/L2·8H2The ethylenediamine tetra-acetic acid of O and 94g/L is according to volume ratio 2:1 mixing, is vigorously stirred 30min make its be uniformly mixed, obtain transparent micro emulsion, then with ammonium hydroxide adjust pH value be 11.4, the ultrasound 14min at 84 DEG C, Ultrasonic power is 20KHz, obtains clear gel, is then washed with distilled water to AgNO3Solution inspection does not measure Cl-, then use Ethanol washing 3 times, the zirconium oxide presoma after washing is put into thermostatic drying chamber, in 60 DEG C of dry 15h;
Step 3 prepares filler A, filler B and filler C
By zirconium oxide presoma, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, and are sufficiently stirred It mixes uniformly, obtains far infrared additive slurry A, be then baked to, under nitrogen protection in 500 DEG C of calcining 3h, pulverize, Up to filler A;
By tourmaline nano particle, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, sufficiently It stirs evenly, obtains anionic additive slurry B, be then baked to, under nitrogen protection in 410 DEG C of calcining 3h, be ground into Powder is to get filler B;
By Nano silver grain, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, and are sufficiently stirred Uniformly, obtain antibacterial additives slurry C, be then baked to, under nitrogen protection in 300 DEG C of calcining 3h, pulverize to get Filler C;
Step 4 prepares polyester master particle
Firstly, filler A, filler B, filler C and ethylene glycol are mixed, ultrasound 5h at room temperature after stirring obtains mixed liquor; Then mixed liquor and p-phthalic acid, catalyst aid are esterified, polymerize, obtains polyester master particle;
Wherein, esterification temperature is 260 DEG C, pressure 280kPa, and polycondensation reaction is carried out when esterification yield reaches greater than 96.5%, is contracted Poly- temperature is 290 DEG C, is evacuated to 20MPa, when polycondensation to inherent viscosity is 0.74 deciliter/gram, discharging, and blank;
Step 5 prepares polyester preoriented yarn
Polyester master particle is melted, filter is then fed into and is filtered, after metering, into spinning pack, then will be sprayed Tow carry out it is cooling, oil, preoriented yarn is wound into after deflector roll, wherein spinning temperature is 285 DEG C, and spinning speed is 3400m/min;
Step 6 prepares polyester complex fiber
Polyester preoriented yarn can be prepared into polyester functional fibre after a roller, hot tank, two rollers, scroll tube, winding, wherein Draft speed is 500m/min, and draw ratio 3.1, a roll temperature is 90 DEG C, and two roll temperatures are 140 DEG C.
The far-infrared radiated property of fiber is characterized by measuring the normal emittance of polyester complex fiber in the present embodiment, Inspection result shows that its normal emittance is 0.73, and quasi- about the assessment of bids of far infrared performance according to this field, normal emittance is greater than Far-infrared textiles can be assessed as equal to 0.8, the composite fibre in the present embodiment does not meet standard requirements;
Measure the anionic property of polyester complex fiber in the present embodiment:
Detected using air ion concentration relative standard's measuring device, the polyester complex fiber that the application is obtained and Conventional polyester fiber is cut into 10 × 10cm respectively2Size, apart from above-mentioned detection device 6.5cm2Air inlet 2mm or so, measurement Negative ion concentration in air, the polyester fiber anion emission number for obtaining the application is 1034 anion/cm3, this implementation The polyester complex fiber anion emission performance of example is to be improved.
Embodiment 3
It is a kind of with magnetism, far infrared, antibacterial functions composite fibre, the composite fibre be a kind of polyester complex fiber, Specifically, the polyester complex fiber using polyester as substrate, using filler A, filler B and filler C as additive, passes through the blended system of melting It is standby to obtain;In terms of content, raw material includes according to weight percent:16% filler A, 4% filler B, 10% filler C, surplus is polyester.
It wherein, is far infrared additive about filler A, filler A, filler A includes:ZrO2Nano-powder and hollow Fe3O4It receives The mass fraction of rice grain, each substance is:ZrO215 parts of nano-powder, hollow Fe3O44 parts of nano particle;The ZrO2Nano-powder Partial size be 20nm, the hollow Fe3O4Nano particle diameter is 250nm;
It wherein, is anionic additive about filler B, filler B, filler B includes:Tourmaline nano particle and hollow Fe3O4The mass fraction of nano particle, each substance is:17 parts of tourmaline nano particle, hollow Fe3O411 parts of nano particle;It is described Tourmaline nano particle diameter be 100nm, the hollow Fe3O4Nano particle diameter is 250nm;
It wherein, is antibacterial additives about filler C, filler C, filler C includes:Nano silver grain and hollow Fe3O4Nanometer The mass fraction of particle, each substance is:10 parts of Nano silver grain, hollow Fe3O47 parts of nano particle;The nano grain of silver seed Diameter is 50nm, the hollow Fe3O4Nano particle diameter is 250nm.
It the following is the preparation process of the polyester complex fiber:
Step 1, dispersing agent is prepared
Weigh FeCl3·6H2O, hexamethylenetetramine, polyvinylpyrrolidone are respectively 1.35g, 0.28g, 0.7g, will be upper It states substance to be successively dissolved in ethylene glycol, forms mixed solution, wherein ethylene glycol volume is 30ml, then magnetic agitation, after stirring The mixed solution is transferred in ptfe autoclave, reaction kettle is put into electric drying oven with forced convection, is protected at 220 DEG C Warm 15h after the reaction was completed takes out reaction kettle, cooled to room temperature, and the powder that reaction obtains is centrifuged, then It is cleaned by ultrasonic with distilled water, powder is then obtained into hollow Fe after 75 DEG C of dry 9h in a vacuum drying oven3O4Nano particle;
Step 2 prepares zirconium oxide presoma
By the ZrOCl of 720g/L2·8H2The ethylenediamine tetra-acetic acid of O and 94g/L is according to volume ratio 2:1 mixing, is vigorously stirred 30min make its be uniformly mixed, obtain transparent micro emulsion, then with ammonium hydroxide adjust pH value be 11.4, the ultrasound 14min at 84 DEG C, Ultrasonic power is 20KHz, obtains clear gel, is then washed with distilled water to AgNO3Solution inspection does not measure Cl-, then use Ethanol washing 3 times, the zirconium oxide presoma after washing is put into thermostatic drying chamber, in 60 DEG C of dry 15h;
Step 3 prepares filler A, filler B and filler C
By zirconium oxide presoma, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, and are sufficiently stirred It mixes uniformly, obtains far infrared additive slurry A, be then baked to, under nitrogen protection in 500 DEG C of calcining 3h, pulverize, Up to filler A;
By tourmaline nano particle, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, sufficiently It stirs evenly, obtains anionic additive slurry B, be then baked to, under nitrogen protection in 410 DEG C of calcining 3h, be ground into Powder is to get filler B;
By Nano silver grain, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, and are sufficiently stirred Uniformly, obtain antibacterial additives slurry C, be then baked to, under nitrogen protection in 300 DEG C of calcining 3h, pulverize to get Filler C;
Step 4 prepares polyester master particle
Firstly, filler A, filler B, filler C and ethylene glycol are mixed, ultrasound 5h at room temperature after stirring obtains mixed liquor; Then mixed liquor and p-phthalic acid, catalyst aid are esterified, polymerize, obtains polyester master particle;
Wherein, esterification temperature is 260 DEG C, pressure 280kPa, and polycondensation reaction is carried out when esterification yield reaches greater than 96.5%, is contracted Poly- temperature is 290 DEG C, is evacuated to 20MPa, when polycondensation to inherent viscosity is 0.74 deciliter/gram, discharging, and blank;
Step 5 prepares polyester preoriented yarn
Polyester master particle is melted, filter is then fed into and is filtered, after metering, into spinning pack, then will be sprayed Tow carry out it is cooling, oil, preoriented yarn is wound into after deflector roll, wherein spinning temperature is 285 DEG C, and spinning speed is 3400m/min;
Step 6 prepares polyester complex fiber
Polyester preoriented yarn can be prepared into polyester functional fibre after a roller, hot tank, two rollers, scroll tube, winding, wherein Draft speed is 500m/min, and draw ratio 3.1, a roll temperature is 90 DEG C, and two roll temperatures are 140 DEG C.
The far-infrared radiated property of fiber is characterized by measuring the normal emittance of polyester complex fiber in the present embodiment, Inspection result shows that its normal emittance is 0.82, and quasi- about the assessment of bids of far infrared performance according to this field, normal emittance is greater than Far-infrared textiles can be assessed as equal to 0.8, the polyester complex fiber in the present embodiment is met the requirements of the standard;
Measure the anionic property of polyester fiber in the present embodiment:
It is detected using air ion concentration relative standard's measuring device, the polyester fiber that the application is obtained and common Polyester fiber is cut into 10 × 10cm respectively2Size, apart from above-mentioned detection device 6.5cm2Air inlet 2mm or so, measure air Middle negative ion concentration, the polyester fiber anion emission number for obtaining the application is 2378 anion/cm3, and conventional polyester The negative ion concentration of fiber is substantially zeroed, illustrates that the polyester complex fiber of the application has good anion emission performance.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (7)

1. it is a kind of with magnetism, far infrared, antibacterial functions composite fibre, the composite fibre be a kind of polyester complex fiber, should Polyester complex fiber is using polyester as substrate, using filler A, filler B and filler C as additive, by melting blended be prepared;Its It is characterized in that, wherein filler A includes:ZrO2Nano-powder and dispersing agent;Filler B includes:Tourmaline nano particle and point Powder;Filler C includes:Nano silver grain and dispersing agent.
2. composite fibre according to claim 1, which is characterized in that in the polyester complex fiber, in terms of content, Raw material includes according to weight percent:16% filler A, 4% filler B, 3% filler C, surplus are polyester.
3. composite fibre according to claim 1, which is characterized in that the dispersing agent is hollow Fe3O4Nano particle, institute State hollow Fe3O4Nano particle is prepared by solvent-thermal method, partial size 250nm.
4. composite fibre according to claim 3, which is characterized in that in the filler A, the mass fraction of each substance is: ZrO215 parts of nano-powder, hollow Fe3O44 parts of nano particle;The ZrO2The partial size of nano-powder is 20nm.
5. composite fibre according to claim 3, which is characterized in that in the filler B, the mass fraction of each substance is: 17 parts of tourmaline nano particle, hollow Fe3O411 parts of nano particle;The tourmaline nano particle diameter is 100nm.
6. composite fibre according to claim 3, which is characterized in that in the filler C, the mass fraction of each substance is: 10 parts of Nano silver grain, hollow Fe3O47 parts of nano particle;The Nano silver grain partial size is 50nm.
7. the composite fibre according to any one of claim 3-6, which is characterized in that the preparation of the polyester complex fiber Process:
Step 1, dispersing agent is prepared
Weigh FeCl3·6H2O, hexamethylenetetramine, polyvinylpyrrolidone are respectively 1.35g, 0.28g, 0.7g, by above-mentioned object Matter is successively dissolved in ethylene glycol, forms mixed solution, wherein ethylene glycol volume is 30ml, then magnetic agitation, should after stirring Mixed solution is transferred in ptfe autoclave, and reaction kettle is put into electric drying oven with forced convection, is kept the temperature at 220 DEG C 15h after the reaction was completed takes out reaction kettle, cooled to room temperature, and the powder that reaction obtains is centrifuged, then uses Distilled water ultrasonic cleaning, then obtains hollow Fe after 75 DEG C of dry 9h in a vacuum drying oven for powder3O4Nano particle;
Step 2 prepares zirconium oxide presoma
By the ZrOCl of 720g/L2·8H2The ethylenediamine tetra-acetic acid of O and 94g/L is according to volume ratio 2:1 mixing, is vigorously stirred 30min It is uniformly mixed it, obtains transparent micro emulsion, then adjusting pH value with ammonium hydroxide is 11.4, ultrasound 14min, ultrasonic function at 84 DEG C Rate is 20KHz, obtains clear gel, is then washed with distilled water to AgNO3Solution inspection does not measure Cl-, then washed with ethyl alcohol It washs 3 times, the zirconium oxide presoma after washing is put into thermostatic drying chamber, in 60 DEG C of dry 15h;
Step 3 prepares filler A, filler B and filler C
By zirconium oxide presoma, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, and are sufficiently stirred It is even, obtain far infrared additive slurry A, be then baked to, under nitrogen protection in 500 DEG C of calcining 3h, pulverize to get Filler A;
By tourmaline nano particle, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, and are sufficiently stirred Uniformly, anionic additive slurry B is obtained, is then baked to, under nitrogen protection in 410 DEG C of calcining 3h, is pulverized, i.e., Obtain filler B;
By Nano silver grain, hollow Fe3O4Nano particle and titanate coupling agent are add to deionized water, and are stirred, Antibacterial additives slurry C is obtained, is then baked to, under nitrogen protection in 300 DEG C of calcining 3h, is pulverized to get filler C;
Step 4 prepares polyester master particle
Firstly, filler A, filler B, filler C and ethylene glycol are mixed, ultrasound 5h at room temperature after stirring obtains mixed liquor;Then Mixed liquor and p-phthalic acid, catalyst aid are esterified, polymerize, obtains polyester master particle;
Wherein, esterification temperature is 260 DEG C, pressure 280kPa, and polycondensation reaction, polycondensation temperature are carried out when esterification yield reaches greater than 96.5% Degree is 290 DEG C, is evacuated to 20MPa, when polycondensation to inherent viscosity is 0.74 deciliter/gram, discharging, and blank;
Step 5 prepares polyester preoriented yarn
Polyester master particle is melted, filter is then fed into and is filtered, after metering, into spinning pack, then by the silk of ejection Shu Jinhang is cooling, oils, and preoriented yarn is wound into after deflector roll, wherein spinning temperature is 285 DEG C, spinning speed 3400m/ min;
Step 6 prepares polyester complex fiber
Polyester preoriented yarn can be prepared into polyester functional fibre after a roller, hot tank, two rollers, scroll tube, winding, wherein drawing-off Speed is 500m/min, and draw ratio 3.1, a roll temperature is 90 DEG C, and two roll temperatures are 140 DEG C.
CN201810591916.7A 2018-06-11 2018-06-11 It is a kind of with magnetism, far infrared, antibacterial functions composite fibre Pending CN108842217A (en)

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