CN102660799A - Nano ZrO2 composite polyester functional fiber, manufacturing method thereof and application - Google Patents

Nano ZrO2 composite polyester functional fiber, manufacturing method thereof and application Download PDF

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CN102660799A
CN102660799A CN2012101734554A CN201210173455A CN102660799A CN 102660799 A CN102660799 A CN 102660799A CN 2012101734554 A CN2012101734554 A CN 2012101734554A CN 201210173455 A CN201210173455 A CN 201210173455A CN 102660799 A CN102660799 A CN 102660799A
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nano
nanometer zro
zro
fiber
nanometer
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周晓地
吴进前
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NANJING LONGYI TEXTILE TECHNOLOGY DEVELOPMENT CO LTD
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NANJING LONGYI TEXTILE TECHNOLOGY DEVELOPMENT CO LTD
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Abstract

A nano ZrO2 composite polyester functional fiber contains ZrO2, polybutylene terephthalate, polyethylene terephthalate and a small quantity of auxiliaries, and is manufactured by means of a novel nano ZrO2 powder dispersing and wrapping process and by adjusting a spinning process. The nano ZrO2 composite polyester functional fiber realizes nano-dispersion of nano ZrO2 in a polyester carrier, hydrolysis of composite polyester master batch preparation and degradation of nano composite master batch in polybutylene terephthalate during secondary melting dispersion, and overcomes the shortcomings of the prior art, so that nano ZrO2 powder particles are uniformly distributed and organically compounded in polyester fibers, and mass production of the fiber is realized. A product made of the fiber can efficiently emit biological infrared waves in a long-acting manner, is ultraviolet-resistant, has the health care function of improving human microcirculation and has a sunscreen effect, and a novel fabric market is certainly activated owing to the advantages of functionality, comfort and variety and color diversity of the fiber.

Description

Nanometer ZrO 2Complex polyester functional fibre and manufacturing approach thereof and application
Technical field
The invention belongs to the new textile material field, relate in particular to a kind of nanometer ZrO 2Complex polyester functional fibre and manufacturing approach thereof and application.
Background technology
Infra-red radiation has big quantity research bibliographical information and extensive use both at home and abroad to organism and medical health care effect and mechanism.Research shows: 9-11 mu m waveband infra-red radiation is easy to absorbed by human body skin, can be used for the warm, health care field; Therefore it is consistent that 10-16 mu m waveband infra-red radiation radio frequency rate and the organic sight of human body can be rolled into a ball the peptide chain eigentone, can cause the resonance of human body cell and produce fuel factor, promotes the infiltration and the absorption of medicine, plays good medical assistance effect; In addition; The infra-red radiation of some specific band scopes can also stimulate the nervous system of human body; Make human body produce a series of physiological reactions, thereby enhances human body is metabolic, improves physical function and improve immunity like visceral motility reinforcement, blood vessel dilatation, blood flow quickening etc.Aspect the research of Chinese medicine meridian and infrared light; Experiment proof: the collaterals of human material is the collagenous fibres of a kind of biological fluids crystalline state (Bio-Liquid Crystal) of being made up of several different proteins molecules; Collagenous fibres are at the light transmittance that radially infrared ray of 9-20 micron is had nearly 100%; Lateral aspects is then almost completely light tight, that is to say in this frequency range, and collaterals of human material collagenous fibres have the physical characteristic of fiber optics.
Therefore, will have low-temperature biological infra red radiation function material and combine, have warming, health care and medical miscellaneous function human body thereby can give textiles with textile material.Correlation technique and application have a large amount of reports; As: Chinese invention patent ZL 96103486.6 discloses a kind of preparation method of far infrared cloth; Be in polypropylene, to add aluminium oxide, titanium oxide, magnesia and zirconia to be in the far-infrared ceramic at least two kinds and to be raw material; Process long filament and further process cloth through spinning and subsequent handling and be processed into the health-care underclothes trousers and have good promotion microcirculation and sanguimotor function, the illness that microcirculation disorder is caused has tangible doing well,improving and supplemental treatment effect; Chinese invention patent publication number CN00100837 discloses a kind of manufacturing approach of fiber of tool far infrared irradiation; Key step is that magnesia, calcium oxide, zirconia, silica, praseodymium and cerium are ground to form 1 micron powder and be mixed and made into the far infrared ceramic powder end; Be dispersed into pre-feed with resin, dispersant and wetting agent via mixing and grinding again; Pre-feed and particles mixed process master batch, mix, utilize the extruder extruding of heating with polyester grain and tool far-infrared matrix through extruder; Make it become molten slurry; Via filter impurity is separated, and after the spinning machine spinning, promptly become a kind ofly have heat storing and heat preserving, stimulate circulation, the fiber of the tool far infrared irradiation of effect such as antibiotic and deodorization.
Closely during the last ten years, along with the develop rapidly of nanometer technology, it is found that infrared ceramic material processed nano particle after, wideization taken place in its infrared emission peak, thereby overlaps better with the biological wave band of human body radiation; In addition, the nanometer particle particle diameter reduces, and scattering coefficient reduces, and its emissivity has also had raising; Simultaneously, particle has higher specific surface, and stronger activity is more firm with the adhesion of polymer support, thereby has desirable compound durability; Therefore adopt nano material to combine with textile technology, nanometer infrared health functional fibre is made in exploitation and lining is the direction of this technical development.But nano material and common material have more excellent physicochemical characteristics; Especially inorganic particle or powder when using because small size reunion factor; Also exist many guardian technique predicaments at present, particularly with polymer macromolecular material compound tense, the nanoscale that how to guarantee particle to greatest extent disperses and is compound; Thereby keeping the nano material excellent specific property, is the problem that current nano material application development must be faced.
The method of making nanometer infrared health functional fibre and lining in theory mainly contains three kinds of approach: (1) cladding process; It is the adhesive that contains the nanometer infrared ceramic powder in the lining surface-coated; The significant disadvantages of this method is to guarantee tack and the stability of nanometer powder at fiber or fabric face, especially the comfortableness of fabric and repeatedly wash lasting effect.(2) composite fibre mother material; Be that nano functional ceramic powder and organic polymer blend are formed the nano-composite fiber masterbatch; Again by a certain percentage with itself and spinning material blend spinning; This method technology, technology and fiber quality operability are good, and key is how to guarantee effectively nano-ceramic powder to be dispersed in the masterbatch with the nano particle state, and technical have a bigger difficulty; Because the natural reunion characteristic certainly of nano material, general various dry blending technology can't address this problem at present.(3) synthetic fiber masterbatch (section) method; It is the big molecule of fiber that original position is synthetic, formation is coated with nano particle that in the presence of nano-powder, carries out fibrous raw material; Constitute the nano-composite fiber masterbatch, again with method spinning with (2), or the direct slicing spinning; The key of this method is that technology, technology and the equipment requirements of synthetic fiber masterbatch is all very complicated and difficult, and cost is relative also very high.
Add the infrared powder body material of nanoscale; Thereby more existing public reported of the application technology of giving fiber and textiles corresponding function thereof; As: Chinese invention patent ZL200510070910.8 discloses a kind of artificial fiber capable of releasing far infrared ray and process for preparing same, and this fiber comprises artificial fibre raw material and nano particle capable of releasing far infrared ray; This method for making provides artificial fibre raw material and nano particle at first respectively, then mixes artificial fibre raw material and nano particle, and makes artificial fibre with the artificial fibre raw material of mix nanoparticles; Wherein this nano particle is a particle capable of releasing far infrared ray, and the far infrared wave-length coverage is from 4 microns to 14 microns; Owing to be nano level particle; Can in artificial fibre, be uniformly dispersed, so the present invention can improve weaving efficient, and absorbed better by human body by the far-infrared engergy that discharges; Make the ICW subactivity more active, and then stimulate circulation and enhance metabolism.Though relating to nano particle, this technology uses; The separation method of nanometer and micron particles is proposed; But how to solve intrinsic the reuniting (generally existing in the air) naturally of nano particle with micron or sub-micro aggregation state; Thereby and combine to bring into play its nano particle effect with organic high score material, and relate to crucial inorganic nano particle and how to combine dispersion not put forward solution with organic polymer with the nano particle state.Chinese invention patent ZL 200410072376.X discloses a kind of manufacturing approach of far infrared-antistatic polyester fiber; Adopt raw material PTA terephthalic acid (TPA) and EG ethylene glycol under the condition of heating, to carry out the BHET ethylene glycol terephthalate monomer material importing polymeric kettle that esterification generates; Add the antistatic additive EG slurries that modulate in the normal pressure polycondensation reaction stage; Keep beginning the polycondensation reaction of reducing pressure behind the certain hour; After reaction finishes the antistatic polyester melt that generates is cooled off the back pelleter with the mode of water-cooled and process the antistatic polyester section: after the antistatic polyester section is mixed with the nano far infrared ceramic powder master batch, be spun into and have far infrared-antistatic complex function polyester staple fiber.This technology has proposed complex functionality static polyester slice method; Although adopt nanometer infra-red china master batch; But just conventional usually dry mixed is processed, and is not nano-dispersed composite master batch truly, and staple fiber spinning disperses to require relatively low to additive in the master batch; The same with aforementioned patent, same not mentioned nano-dispersed complex method.
ZrO 2Material non-toxic, "dead"; Owing to its material composition and crystal structure have special low temperature infrared emission performance (particular organisms infrared band and high radiant rate); Be used for polymer fiber lining and fabric; Have and improve human body skin microcirculation and the effect that improves shell temperature, should have vast potential for future development at the thermal insulation of human body and medical health field.This material has higher emissivity in about 3-25 μ m infrared band at low temperatures, with ZrO 2After processing nano particle, wideization and " blue shift " have taken place in its infrared emission peak, thereby overlap better with biological infrared a few to tens of micron wavebands of human body, and the nanometer materials emissivity has also had raising, can reach 93%, even higher.Therefore, nanometer ZrO 2Be a kind of desirable biological infrared health fiber and the compound interpolation material of function of lining; Especially it is the biological efficiently infrared emission material of a kind of single-component low temperature; Used function is added material in the above-mentioned listed technology also has this composition of employing; But generally be non-nanoscale, and all be one of group's part composition but not main component that its good characteristic does not obtain fully effectively utilizing.Chinese invention patent ZL200710118929.4 discloses a kind of nano composite polyester functional fibre and manufacturing approach and application; Its fiber contains weight portion nano-ceramic powder 12-45 part, polipropene 25 0-270 part and Tissuemat E 2-18 part; Fibre single thread fiber number 0.5-1.5D; Fracture strength is processed through steps such as the dispersion of nano-ceramic powder water, pre-dispersed presoma, composite master batch, compound slice and high speed spinnings greater than 2.5cN/dtex.Said nano ceramics meal component is ZrO 2Or ZrO 2With ZrC, TiO 2And Ag +In the antiseptic one or more, ZrO wherein 2Be not less than 2 parts, its particle diameter and in composite master batch and fiber decentralization less than 100nm.Adopt this fiber to can be made into various multifunctional textile article; As: CRUX dress ornament, underwear, bedding, shirt, socks and various protector goods etc.; Have the sub-energy of the emitting biological glistening light of waves, uvioresistant, antibiotic, absorb and intercept near infrared ray and multiple functions such as wet are led in perspire, thereby give antibacterial textile health, energy health care, heat insulation sun, heat storing and heat preserving, dry and comfortable multiple function such as comfortable.This technology is with nanometer ZrO 2As the characteristic functional component; And adopted unique water to disperse and coating technology; Having solved reunion depolymerization and the organic scattering problem of nano material in application well, is the most economic, the effective inorganic nano material composite fibre manufacturing technology of issue at present.However; This technology also has its obvious limitation; Though polypropylene polypropylene fiber and lining have its unique application, its difficult dyeing, lower fusing point make it mix with other fibrous material and put in order after woven and finalize the design limitedly, seriously restrict its application; And the polyester fiber in the three big synthetic fiber does not have the problem of this respect, has more application prospects and market; Owing to adopt aqueous medium and heating means, it is suitable for not absorbing water, to the organic-inorganic nano composition operation of insensitive, the nonpolar polypropylene based material of water as carrier in the above-mentioned technical process, and is satisfactory for result; But to hydrophilic, the polyester of polarity, polyamide-based material; Especially be responsive polyester to water electrode under the high temperature, above-mentioned technology does not propose effective solution as yet, therefore; The nano composite polyester infrared health functional fibre for preparing real function admirable; And and then process lining, thereby realize comfortableness, popularity that the functional fibre lining is used, some key problem in technology and difficult point wait solution.
Summary of the invention
The technical problem that the present invention will solve is: overcome the above-mentioned deficiency of prior art, a kind of nanometer ZrO is provided 2Complex polyester functional fibre and manufacturing approach thereof, it passes through nanometer ZrO 2The powder liquid phase is disperseed and organic coating, the presoma that anhydrates preparation, composite master batch preparation, master batch secondary mixed and dispersed, and new technology operations such as composite spinning are processed the nano composite polyester functional fibre, wherein ZrO 2Particle diameter is 10-60nm.The invention solves nano compound agglomerate moisture content problem and the nano compound agglomerate degradation problem during the secondary mixed and dispersed in PET, solved defective of the prior art and deficiency.Thereby realized that the nano-powder particle evenly distributes in polyester fiber; And it is organic compound with polyester fiber; The spinnability of composite function nano fiber, thin dawnization and kind, color variation degree are improved greatly, for the volume production of nano compound polyester fibre has been paved road.Through " country infrared and industrial electroheat product quality supervision inspection center " and " national cotton textile quality monitoring inspection center " detection, the comfortable softness of this product lining meets the practicability standard; Have long-acting emissive porwer 87% biological infrared waves function and the effect that increases microcirculation in human body 15.27%, and have ultraviolet protection function (absorptivity 99.82%); Market prospects are extensive, adopt this fiber and lining to can be made into various health cares, sun-proof, heat insulation function textiles, as: CRUX dress ornament, underwear, bedding, shirt and various protector goods.
In order to solve above technical problem, nanometer ZrO provided by the invention 2The complex polyester functional fibre is characterized in that: this fiber contains the following raw materials according component:
Nanometer ZrO 2Powder: 3~7 weight portions
Polybutylene terephthalate: 2~20 weight portions
PET: 70~95 weight portions
Auxiliary agent: trace;
Said nanometer ZrO 2Powder directly is 10-100nm;
With above-mentioned nanometer ZrO 2Powder disperses through water, processes the water-soluble colloidal state slurry of nano-dispersed, and then mixes with solvent naphtha, forms water, oily two phase blended liquid phase systems, and through the suitable adjuvants effect, behind chemical reaction, the product drying becomes the organic coating presoma that anhydrates; This presoma is mixed parcel with the polybutylene terephthalate particle, prepare composite master batch through the kneader fusion again, behind PET secondary mixed and dispersed melt spinning, form nanometer ZrO 2The complex polyester functional fibre.
The further technical characterictic of the present invention also is:
1, said nanometer ZrO 2The filament number 0.5-2D of complex polyester functional fibre, fibrous fracture intensity is greater than 3.0cN/dtex; The particle diameter of the nano powder that is adopted and the average mark divergence in composite master batch and composite functional fiber thereof are less than 100nm.
2, said a spot of auxiliary agent comprises anion surfactant and cationic surfactant reaction afterproduct and ethylene-acrylic acid copolymer; Said anion surfactant is a fatty acid ester sulfonate, and said cationic surfactant is a rosin amine; Said auxiliary agent content is nanometer ZrO 2The 5-15% of weight.
In addition, the present invention also provides a kind of preparation nanometer ZrO 2The method of complex polyester functional fibre is characterized in that this method comprises the steps:
1) nanometer ZrO 2The powder water disperses: with the nanometer ZrO of 3~7 weight portions 2Powder, anion surfactant and water are processed the water-soluble colloidal state ceramic size of nano-dispersed that concentration is 20~40wt% through ball milling or sand milling at normal temperatures; Described anion surfactant consumption is 6~12wt% of nano ceramics weight;
2) the nano particle liquid phase coats: the ethylene-acrylic acid copolymer and the solvent naphtha that in water, add nano powder weight 5~15wt% stir, and form the oil phase system in 60~95 ℃ of following water; The water-soluble colloidal state ceramic size of nano-dispersed in the step 1) is joined in this oil phase system,, form water, oily two phase blended liquid phase systems through stirring; Add cationic surfactant then, anion surfactant, cationic surfactant combine to form the organic coating product of nano particle with ethylene-acrylic acid copolymer behind chemical reaction; The consumption of cationic surfactant, solvent naphtha and water is by nano powder weight, is respectively, 6~12wt%, 20~50wt% and 10~30 times;
3) anhydrate presoma preparation and mixed once: with step 2) obtain the organic coating product of nano particle and anhydrate through drying; Anhydrate product and weight portion of gained is that 2~20 parts polybutylene terephthalate particle is made mixed once in high-speed mixer; Form nano combined presoma enwrapped granule, it is subsequent use to be cooled to room temperature after the oven dry;
4) nanometer ZrO 2Composite master batch preparation: the nano combined presoma enwrapped granule of step 3) gained is descended through the screw extruder fusions at 230~260 ℃, mediates, extrudes, process nanometer ZrO 2The complex polyester master batch;
5) the secondary mixed and dispersed of spinning material: with the nanometer ZrO for preparing in the step 4) 2Composite master batch drying again anhydrates, with weight portion be that 70~95 parts PET is made the secondary mixed and dispersed;
6) nanometer ZrO 2Composite polyester fiber spinning: nanometer ZrO 2Composite master batch and PET secondary mixed and dispersed are after melt spinning and deformation technique are processed nanometer ZrO 2The complex polyester functional fibre.
It is thus clear that the related auxiliary agent of the present invention plays the effect of a bridge in the preparation method, inorganic matter and organic matter are combined.Auxiliary agent (low molecule) is extruded to spinning material (macromolecule) in screw rod HTHP extrusion an appearance and a part are filtered product (the nanometer ZrO that is therefore finally obtaining 2The complex polyester functional fibre) in, auxiliary agent has only minimal residue.
Said anion surfactant is a fatty acid ester sulfonate, and said cationic surfactant is a rosin amine.
In the step 3) of the inventive method; The drying of the organic coating product of nano particle and the oven dry of nano combined presoma enwrapped granule are all carried out in negative pressure hydrofuge drying system; The temperature of said negative pressure hydrofuge drying system is 60-90 ℃; Pressure limit is a 0.5-0.8 atmospheric pressure, and drying time is no less than 24 hours; In the said step 5), nanometer ZrO 2The baking temperature of complex polyester master batch is 60-90 ℃, and is dry more than 24 hours.
In the step 5), nanometer ZrO 2Complex polyester master batch secondary mixes in the preheating zone be dispersed in the spinning screw case and carries out, and in the step 6), melt temperature is 260~280 ℃, and spinning temperature is 280~300 ℃, and spinning speed is 2300~3200m/s.
Adopt functional fibre provided by the invention can process various linings or fabric, it is characterized in that: the said nanometer ZrO of all or part of employing claim 1 2At least a mixed textile in complex polyester functional fibre and cotton, fiber crops, silk, polyamide fibre, spandex, cellulose fibre, the wood pulp fibre forms, wherein nanometer ZrO 2Complex polyester functional fibre content is not less than 25wt%.
And the present invention also provides described nanometer ZrO 2Complex polyester functional fibre application process; It is characterized in that: that adopts that part or all of this fiber can be made into has emitting biological infrared waves, a uvioresistant, is used to keep healthy, CRUX dress ornament, underwear, bedding, shirt, socks and the various protector goods of sun-proof, insulation.
The present invention compared with prior art has the following advantages and the high-lighting effect:
1. the nanometer ZrO of the preferred one-component of the present invention 2Powder body material is infrared functional additive; Composition is simple, raw material sources are abundant, controlled; Have the biological infrared waves emissivities of 2~25 high μ m under this material normal temperature, radiance preferably can reach more than 95% greater than 90%; More than requiring its emissivity of adding functional component 80% to want high to infrared functional fibre in the prior art; Also having good uvioresistant and absorption near infrared ray characteristic simultaneously, is the infrared functional material of a kind of good nano biological, can guarantee the efficient functional characteristic that its composite fibre is good.In addition, nanometer ZrO 2Color is for being white or translucent white; Can keep fiber true qualities or shallow white after processing fiber, its lining and fabric have broad spectral range in follow-up dyeing is handled, satisfy the requirement of textile product shades of colour style basically; And existing infrared functional fibre generally all is to adopt many components composition for reaching performance requirement; Generally all be coloured, its fiber of processing also is coloured, therefore is difficult to satisfy follow-up various actual instructions for use.Select nanometer ZrO 2, be because its particular chemical composition and structures shape, according to quantum-mechanical theory, dipole moment changes more greatly in the molecular vibration process, and absorption band is strong more accordingly, and radiation is strong more, and the size of dipole moment (being degree of polarization) is directly proportional nanometer ZrO with polarizability 2It is relevant with elastic displacement polarization (comprising the electron displacement polarization and the ion displacement polarization of the ion) characteristic of its crystal to have high biological infrared emittance; The electron displacement polarization degree of ion is except relevant with its polarizability size; Also relevant with the size of ion; Zirconium is all bigger than the ionic radius of silicon, aluminium, titanium etc., ZrO 2Crystal intermediate ion displacement polarization ability also is eager to excel, and dipole moment changes greatly, and its radiation absorbs also stronger relatively, thereby is desirable photon energy radiative material; Simultaneously because the nanoscale of its structure, thereby have good spectral absorption characteristics, can effectively absorb ultraviolet ray and near-infrared heat ray.
2. the nanoscale ZrO that adopts of the present invention 2Powder body material all is a synthetic material, has effectively guaranteed the functional of its reliable security and excellence.But synthetic material preferred raw material and technology are effectively controlled material composition, purity, avoid introducing harmful substance; When material reaches nanoscale, because of it has very small dimensions and very big surface area, the increase of material surface atomicity relative scale; Monoatomic surface energy improves rapidly, and the variation of this form feeds back on the structure of matter and the performance, will show unusual effect; I.e. " nano effect "; As: the variation of the spectral characteristic of material, thereby " blue shift " and " wideization " phenomenon of generation spectral absorption and radiation frequency or wavelength, the also corresponding raising of intensity; The raising of the surface energy of material; The surface atom of particle is more active; Thereby cause that chemism strengthens, not only make the corresponding function material adsorptivity, inhale functional characteristic such as ripple rate and significantly improve, and the functional component of its required interpolation of functional nano composite fibre of processing also can obviously reduce; Thereby improve goods yield rate, economy, and help keeping or improving the traditional performance of composite fibre.
3. the invention provides and solve the process for dispersing of nano material in the polarity polyester material so far the most cost-effectively, especially solved nanometer ZrO 2The spinnability of composite polyester fiber and yield rate problem.Because nano particle has high surface energy and activity; Particularly in air, have under the situation that polar water molecules exists, very easily take place self to reunite or assemble with the hydrone effect, become the non-nano yardstick than macro aggregate; If can not be effectively with its dispersion and stable; Not only influence the performance of its nano effect, also be difficult in evenly dispersion and effectively interpolation in the organic high molecular polymer, thereby have a strong impact on the functional and conventional physical property of composite and fiber owing to it becomes bigger inorganic matter aggregate; Present technology; Comprise that some carry out high-speed stirred, molten surface treatment method such as mix with dry method such as organic dispersing agent, coupling agents, all can not effectively address these problems, can't really accomplish the even dispersion of nanoscale.The existing wet method aqueous dispersion organic coating method that adopts in the prior art, it can solve nanoparticulate dispersed problem in the polypropylene material, but owing to dispersion, coating, recombination process are carrying out in water all the time; Therefore be not suitable for the polarity polyester material; This type material possess hydrophilic property is prone to suction, though can remove a large amount of free waters through desciccate; But the bound water in the middle amalgam is difficult to remove, and polyester will be owing to the existence of these bound water is degraded when follow-up high temperature melting granulation.No matter next step spinning is master batch mixing method or hybrid slicing method, facts have proved at all and can't carry out.The present invention provides a kind of innovative approach; Earlier disperse organic coating product drying to anhydrate water; And then mix parcel with the master batch vector resin; Two-stage process is separately handled; Product is outer self not to absorb water for scolding the low molecular organic Wax of water owing to coat, and is easy to anhydrate; So just can efficiently solve the problem that the intermediate mixture before the high temperature found grain is brought moisture into, avoid the high-temperature water degraded of polyester support.Facts have proved, adopt above-mentioned measure and suitable technology, select and prescription in conjunction with carrier provided by the invention and auxiliary agent, follow-up spinning is smooth, and fibre property is good, and by the requirement of general fibre conventional index, the Grade A productive rate can reach more than 85%.
4. characteristics of the present invention are that also preferred a kind of low-melting point polyester material polybutylene terephthalate is as nanometer ZrO 2The carrier of composite functional fiber masterbatch; All adopting the polyethylene terephthalate materials consistent with the polyester fiber carrier in the prior art is the master batch carrier; The former fusing point is 225~260 ℃, is starkly lower than 265~280 ℃ of the latter, and its water imbibition and high temperature are also good than the latter to water sensitivity; Two kinds of material structures are close with performance, and good mutual fusibleness is arranged.Because adding nano functional particle employing polyester material polybutylene terephthalate is the composite master batch carrier; Its melting extrusion temperature is 225~260 ℃, and PET is the composite master batch carrier, and its melting extrusion temperature needs up to being 285~300 ℃; The latter's cost is obvious more on the low side than the former; Therefore, no matter from technological operation property, product yield and economic benefit, or aspects such as social benefit such as energy-conserving and environment-protective; The present invention provides a kind of excellent technique scheme, embodies tangible advantage.
5. the present invention also is with technological at present difference: composite fibre of the present invention and lining thereof can satisfy people to greatest extent for the requirement of textile product style varied; Present health care textiles because the prescription and manufacturing technology limit; No matter be kind, color, feel and the comfortableness of fiber and lining, or functional effect all has tangible limitation; Adopt the inventive method, can make the polyester fiber of multi-size, comprise high performance fine count fiber.Nanometer ZrO 2The advantage of composite polyester fiber on stainability, high epistasis, high-temperature stability and price; The above-mentioned limitation of existing in prior technology all can be resolved; Its special nanometer composite technology has guaranteed efficient, the permanence of function effectively; Be fit to its and other textile raw material,, adopt woven, knitting and technology mixing such as warp volume is weaved like combinations such as cotton, polyamide fibre, spandex, wool, silk, regenerated fibers; Can process the textile product of various styles requirements and kind; Comprise: CRUX dress ornament, underwear, bedding, shirt, socks and various protector etc., so the present invention has tangible advance, practicality and good market prospects widely will contribute for fabric industry development and human health cause.
Description of drawings
Fig. 1 prepares the method process chart of nano composite polyester functional fibre for the present invention.
The specific embodiment
The present invention adopts nanometer ZrO 2Powder body material is biological infrared functional additive, is that masterbatch carrier, PET are fiber carrier with the polybutylene terephthalate, selects proper assistant for use, processes nanometer ZrO 2The complex polyester functional fibre, each weight portion prescription of forming is 3~7 parts of nanometer ZrO in the fiber 2Powder (particle diameter is 10-100nm), 2~20 parts of polybutylene terephthalates, 70~95 parts of PETs.Through above-mentioned preferred nanometer ZrO 2Powder, nano particle water disperse, the nano particle liquid phase coats, presoma preparation and processing, composite master batch preparation and obtain nanometer ZrO through the composite spinning process 2The complex polyester functional fibre; This fiber of all or part of employing and other general fibre are made into various linings like mixing such as cotton, fiber crops, silk, polyamide fibre, spandex, cellulose fiber peacekeeping wood pulp fibres, wherein nanometer ZrO 2Composite functional fiber content is not less than 25%; Lining or fabric can efficiently be launched the biological infrared waves of 2-25 μ m; But act on health-care functions such as human body warming, a microcirculation improvement; And have anti-ultraviolet sun-proof protection effect, be applicable to and make CRUX dress ornament, underwear, bedding, shirt and various protector goods.
Prepare nanometer ZrO like Fig. 1 for the present invention 2The method process chart of complex polyester functional fibre.
Embodiment 1:
Nanometer ZrO 2The complex polyester functional fibre, 3 parts of nanometer ZrO of components by weight percent prescription 2, 2 parts of polybutylene terephthalates, 95 parts of PETs and little auxiliary, wherein nanometer ZrO 2Powder directly is 10-50nm.At first, 3 parts of nanometer ZrO of weighing 2Powder, oleic acid ethyl ester potassium sulfonate and the water of the 10wt% of interpolation powder weight, it is the aqueous dispersion slurry of 20wt% that ball milling 24hr obtains concentration; Add ethylene-acrylic acid copolymer and No. 120 solvent naphthas of the 15wt% of powder weight in the water, the consumption of solvent naphtha and water is respectively nanometer ZrO 2The 30wt% of grain weight amount and 20 times add above-mentioned slurry down at 80-95 ℃ and stir, and form water, oily two phase blended liquid phase systems; Add the rosin amine of grain weight amount 10wt% then; Through chemical reaction, nano particle coats and the entering oil phase from aqueous phase separation and by copolymer, volatilizes solvent naphtha at 95 ℃ of following constant temperature 2hr; Be cooled to again below 60 ℃ and take out, obtain the nanometer ZrO that anhydrates at 60-90 ℃ of following negative pressure (0.5-0.8 atmospheric pressure) removal moisture drying 36hr 2The presoma of organic coating; This presoma mixes parcel with 2 parts of polybutylene terephthalate particles of weight in high-speed mixer; Enwrapped granule low temperature drying 24hr (the baking temperature scope is 60-90 ℃); After the cooling; Under 240 ℃ through the screw extruder fusion, mediate, extrude and operations such as pelletizing, process the nano composite polyester master batch; Cooperate 95 parts of PETs sections of weight to mix in spinning screw case preheating zone this master batch, carrying out melt spinning subsequently, melt temperature is 260 ℃, and spinning temperature obtains the nanometer ZrO that component requires for being 2300m/s at 280 ℃, spinning speed 2Composite functional fiber, fiber dimensious 75D/72f (filament number 1.0D), intensity is greater than 3.0cN/dtex.Through detecting, the auxiliary agent residual volume is nanometer ZrO 25% of powder.Employing contains this functional fibre of 45wt% and the cotton knitting cloth of 55wt% is processed men and women's T-shirt goods; Test detects: its fabric lining; Normal temperature is the biological infrared waves of emission 2-25 μ m down, and its all band emissivity reaches 87% respectively, and the spf value of uvioresistant A, B is 40+.
Embodiment 2:
Nanometer ZrO 2The complex polyester functional fibre, 4 parts of nanometer ZrO of components by weight percent prescription 2, 10 parts of polybutylene terephthalates, 85 parts of PETs and appropriate amount of addition agent, wherein nanometer ZrO 2Powder directly is 30-60nm.By the fibrous requirement part ZrO that weighs respectively 24 parts in powder, cocoa oleic acid ethyl ester sodium sulfonate and the water of the 12wt% of interpolation nano powder weight stir the aqueous dispersion slurry that 24hr obtains 20wt%; Ethylene-acrylic acid copolymer and No. 100 solvent naphthas of adding the 10wt% of powder weight in the water respectively; The consumption of solvent naphtha and water is respectively 40wt% and 20 times of grain weight amount; Process and embodiment 1 same reaction, coating processing technological flow; Process organic coating presoma that drying is anhydrated, the addition of rosin amine is ZrO in this process 212wt%, then itself and 10 parts of polybutylene terephthalates of weight are mixed parcel in high-speed mixer, in like manner through drying once more, under 260 ℃ through the double screw extruder fusion, mediate, extrude and pelletizing, process the complex polyester master batch; 85 parts of PETs sections of this master batch and weight mix in spinning screw case preheating zone, are carrying out melt spinning subsequently, and melt temperature is 270 ℃, and spinning temperature obtains the nanometer ZrO of component requirement for being 3000m/s at 290 ℃, spinning speed 2Composite functional fiber, fiber dimensious 100D/72f (filament number 1.3), fibre strength 3.2cN/dtex.Through detecting, the auxiliary agent residual volume is nanometer ZrO 210% of powder.Employing contains this functional fibre of 35wt% and the woven lining of drifting of five piece of three shuttle of 65wt% days silks, receives the favorable comment of certain listed company.Test detects: have long-acting emissive porwer 87% biological infrared waves function and the effect that increases microcirculation in human body 15.27%.
Embodiment 3:
Nanometer ZrO 2The complex polyester functional fibre, 7 parts of nanometer ZrO of components by weight percent prescription 2, 20 parts of polybutylene terephthalates, 70 parts of PETs and appropriate amount of addition agent, wherein nanometer ZrO 2Powder directly is 50-100nm.By the fibrous requirement part ZrO that weighs respectively 27 parts in powder, cocoa oleic acid ethyl ester sodium sulfonate and the water of the 6wt% of interpolation grain weight amount stir the nanometer aqueous dispersion slurry that 48hr obtains 40wt% respectively; Ethylene-acrylic acid copolymer and No. 120 solvent naphthas of adding the 5wt% of powder weight in the water respectively; The consumption of solvent naphtha and water is respectively 40wt% and 30 times of grain weight amount; Process and embodiment 1 same reaction, coating processing technological flow; Process organic coating presoma that drying is anhydrated, the addition of rosin amine is ZrO in this process 2The 6wt% of weight mixes parcel with itself and 20 parts of polybutylene terephthalates then in high-speed mixer, in like manner through drying once more, under 230 ℃ through the double screw extruder fusion, mediate, extrude and pelletizing, process the complex polyester master batch; This master batch mixes in spinning screw case preheating zone with the section of 70 parts of PETs, is carrying out melt spinning subsequently, and melt temperature is 280 ℃, and spinning temperature obtains the nanometer ZrO of component requirement for being 3200m/s at 300 ℃, spinning speed 2Composite functional fiber, and fiber dimensious 30D/16f (filament number/2d), intensity 3.5cN/dtex.Through detecting, the auxiliary agent residual volume is nanometer ZrO 215% of powder.It is that product is used in nexine and the 67% cotton parts such as socks and protecting ware for sports that directly are made into for outer and 8% spandex that employing contains this functional fibre of 25wt%; Its more infrared warm-heat effect not only significantly promotes thermal insulation effects such as local joint; More local blood circulation and microcirculation be can strengthen, rehabilitation and medical assistance effect played.
Embodiment 4:
Nanometer ZrO 2The complex polyester functional fibre, 3 parts of nanometer ZrO of components by weight percent prescription 2, 3 parts of polybutylene terephthalates, 90 parts of PETs and appropriate amount of addition agent, wherein nanometer ZrO 2Powder directly is 20-80nm.By the fibrous requirement part ZrO that weighs respectively 23 parts in powder, oleic acid ethyl ester potassium sulfonate and the water of the 8wt% of interpolation nano powder weight stir the aqueous dispersion slurry that 24hr obtains 20wt%; Ethylene-acrylic acid copolymer and No. 100 solvent naphthas of adding the 15wt% of powder weight in the water respectively; The consumption of solvent naphtha and water is respectively 30wt% and 20 times of grain weight amount; Process and embodiment 1 same reaction, coating processing technological flow; Process organic coating presoma that drying is anhydrated, the addition of rosin amine is ZrO in this process 28wt%, then itself and 3 parts of polybutylene terephthalates of weight are mixed parcel in high-speed mixer, in like manner through drying once more, under 260 ℃ through the double screw extruder fusion, mediate, extrude and pelletizing, process the complex polyester master batch; 90 parts of PETs sections of this master batch and weight mix in spinning screw case preheating zone, are carrying out melt spinning subsequently, and melt temperature is 270 ℃, and spinning temperature obtains the nanometer ZrO of component requirement for being 3000m/s at 290 ℃, spinning speed 2Composite functional fiber, fiber dimensious 100D/96f (filament number 1.), intensity 3.0cN/dtex.Through detecting, the auxiliary agent residual volume is nanometer ZrO 28% of powder.Employing contains this functional fibre of 35wt% and textile five piece of three shuttle of 65wt% is woven, the lining jacquard weave, and feel is splendid.Test detects: fabric lining normal temperature is the biological infrared waves of emission 2-25 μ m down, and its all band emissivity reaches 87%.
Embodiment 5:
Nanometer ZrO 2The complex polyester functional fibre, 5 parts of nanometer ZrO of components by weight percent prescription 2, 15 parts of polybutylene terephthalates, 90 parts of PETs and appropriate amount of addition agent, wherein nanometer ZrO 2Powder directly is 10-50nm.By the fibrous requirement part ZrO that weighs respectively 25 parts in powder, cocoa oleic acid ethyl ester sodium sulfonate and the water of the 8wt% of interpolation grain weight amount stir the nanometer aqueous dispersion slurry that 48hr obtains 25wt% respectively; Ethylene-acrylic acid copolymer and No. 120 solvent naphthas of adding the 10wt% of powder weight in the water respectively; The consumption of solvent naphtha and water is respectively 40wt% and 30 times of grain weight amount; Process and embodiment 1 same reaction, coating processing technological flow; Process organic coating presoma that drying is anhydrated, the addition of rosin amine is ZrO in this process 2The 10wt% of weight mixes parcel with itself and 15 parts of polybutylene terephthalates then in high-speed mixer, in like manner through drying once more, under 230 ℃ through the double screw extruder fusion, mediate, extrude and pelletizing, process the complex polyester master batch; This master batch mixes in spinning screw case preheating zone with the section of 90 parts of PETs, is carrying out melt spinning subsequently, and melt temperature is 270 ℃, and spinning temperature obtains the nanometer ZrO of component requirement for being 3000m/s at 290 ℃, spinning speed 2Composite functional fiber, and fiber dimensious 60D/48f (filament number/1.2d), intensity 3.0cN/dtex.Through detecting, the auxiliary agent residual volume is nanometer ZrO 212% of powder.Employing contains this functional fibre of 100wt% and spandex is knitted into slim stamp muffler, and ultraviolet radiation protective effect SPF is greater than 40+, and effect is splendid.
Embodiment 6:
Nanometer ZrO 2The complex polyester functional fibre, 3 parts of nanometer ZrO of components by weight percent prescription 2, 12 parts of polybutylene terephthalates, 80 parts of PETs and appropriate amount of addition agent, wherein nanometer ZrO 2Powder directly is 10-50nm.By the fibrous requirement part ZrO that weighs respectively 23 parts in powder, cocoa oleic acid ethyl ester sodium sulfonate and the water of the 10wt% of interpolation nano powder weight stir the aqueous dispersion slurry that 24hr obtains 30wt%; Ethylene-acrylic acid copolymer and No. 100 solvent naphthas of adding the 10wt% of powder weight in the water respectively; The consumption of solvent naphtha and water is respectively 30wt% and 20 times of grain weight amount; Process and embodiment 1 same reaction, coating processing technological flow; Process organic coating presoma that drying is anhydrated, the addition of rosin amine is ZrO in this process 210wt%, then itself and 12 parts of polybutylene terephthalates of weight are mixed parcel in high-speed mixer, in like manner through drying once more, under 260 ℃ through the double screw extruder fusion, mediate, extrude and pelletizing, process the complex polyester master batch; 80 parts of PETs sections of this master batch and weight mix in spinning screw case preheating zone, are carrying out melt spinning subsequently, and melt temperature is 270 ℃, and spinning temperature obtains the nanometer ZrO of component requirement for being 2500m/s at 300 ℃, spinning speed 2Composite functional fiber, fiber dimensious 75D/144f (filament number 0.5.), intensity 3.0cN/dtex.Through detecting, the auxiliary agent residual volume is nanometer ZrO 25% of powder.Employing contains this functional fibre of 40wt% and textile five piece of three shuttle of 60wt% is woven, and lining is soft, and feel is splendid.Test detects: fabric lining normal temperature is the biological infrared waves of emission 2-25 μ m down, and its all band emissivity reaches 86%.
Except that the foregoing description, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.

Claims (9)

1. nanometer ZrO 2The complex polyester functional fibre is characterized in that: this fiber contains the following raw materials according component:
Nanometer ZrO 2Powder: 3~7 weight portions
Polybutylene terephthalate: 2~20 weight portions
PET: 70~95 weight portions
Auxiliary agent: trace;
Said nanometer ZrO 2Powder directly is 10-100nm;
With above-mentioned nanometer ZrO 2Powder disperses through water, processes the water-soluble colloidal state slurry of nano-dispersed, and then mixes with solvent naphtha, forms water, oily two phase blended liquid phase systems, and through the suitable adjuvants effect, behind chemical reaction, the product drying becomes the organic coating presoma that anhydrates; This presoma is mixed parcel with the polybutylene terephthalate particle, prepare composite master batch through the kneader fusion again, behind PET secondary mixing melt spinning, form nanometer ZrO 2The complex polyester functional fibre.
2. nanometer ZrO according to claim 1 2The complex polyester functional fibre is characterized in that: filament number is 0.5-2D, and fibrous fracture intensity is greater than 3.0cN/dtex; The nanometer ZrO that is adopted 2The particle diameter of powder and the average mark divergence in composite master batch and composite functional fiber thereof are less than 100nm.
3. nanometer ZrO according to claim 1 2The complex polyester functional fibre is characterized in that: said auxiliary agent comprises anion surfactant and cationic surfactant reaction afterproduct and ethylene-acrylic acid copolymer, and said auxiliary agent content is nanometer ZrO 2The 5-15% of weight.
4. nanometer ZrO according to claim 3 2The complex polyester functional fibre is characterized in that: said anion surfactant is a fatty acid ester sulfonate, and said cationic surfactant is a rosin amine.
5. one kind prepares nanometer ZrO 2The method of complex polyester functional fibre is characterized in that this method comprises the steps:
1) nanometer ZrO 2The powder water disperses: with the nanometer ZrO of 3~7 weight portions 2Powder, anion surfactant and water are processed the water-soluble colloidal state ceramic size of nano-dispersed that concentration is 20~40wt% through ball milling or sand milling at normal temperatures; Described anion surfactant consumption is nanometer ZrO 26~12wt% of grain weight amount;
2) the nano particle liquid phase coats: the ethylene-acrylic acid copolymer and the solvent naphtha that in water, add nano powder weight 5~15wt% stir, and form the oil phase system in 60~95 ℃ of following water; The water-soluble colloidal state ceramic size of nano-dispersed in the step 1) is joined in this oil phase system,, form water, oily two phase blended liquid phase systems through stirring; Add cationic surfactant then, anion surfactant, cationic surfactant combine to form the organic coating product of nano particle with ethylene-acrylic acid copolymer behind chemical reaction; The consumption of cationic surfactant, solvent naphtha and water is by nano powder weight, is respectively 6~12wt%, 20~50wt% and 10~30 times;
3) anhydrate presoma preparation and mixed once: with step 2) obtain the organic coating product of nano particle and anhydrate through drying; Anhydrate product and weight portion of gained is that 2~20 parts polybutylene terephthalate particle is made mixed once in high-speed mixer; Form nano combined presoma enwrapped granule, it is subsequent use to be cooled to room temperature after the oven dry;
4) nanometer ZrO 2Composite master batch preparation: the nano combined presoma enwrapped granule of step 3) gained is descended through the screw extruder fusions at 230~260 ℃, mediates, extrudes, process nanometer ZrO 2The complex polyester master batch;
5) the secondary mixed and dispersed of spinning material: with the nanometer ZrO for preparing in the step 4) 2Composite master batch drying again anhydrates, with weight portion be that 70~95 parts PET is made the secondary mixed and dispersed;
6) nanometer ZrO 2Composite polyester fiber spinning: nanometer ZrO 2Composite master batch and PET secondary mixed and dispersed are after melt spinning and deformation technique are processed nanometer ZrO 2The complex polyester functional fibre.
6. according to the said preparation nanometer of claim 5 ZrO 2The method of complex polyester functional fibre; It is characterized in that: in the said step 3); The drying of the organic coating product of nano particle and the oven dry of nano combined presoma enwrapped granule are all carried out in negative pressure hydrofuge drying system; The temperature of said negative pressure hydrofuge drying system is 60-90 ℃, and pressure limit is a 0.5-0.8 atmospheric pressure, and drying time is no less than 24 hours; In the said step 5), nanometer ZrO 2The baking temperature of complex polyester master batch is 60-90 ℃, and is dry more than 24 hours.
7. according to the said preparation nanometer of claim 7 ZrO 2The method of complex polyester functional fibre is characterized in that: in the step 5), and nanometer ZrO 2Complex polyester master batch secondary mixes in the preheating zone be dispersed in the spinning screw case and carries out, and in the step 6), melt temperature is 260~280 ℃, and spinning temperature is 280~300 ℃, and spinning speed is 2300~3200m/s.
8. the described nanometer ZrO of claim 1 2The complex polyester functional fibre is characterized in that: at least a mixed textile in this fiber of all or part of employing and cotton, fiber crops, silk, polyamide fibre, spandex, cellulose fibre, the wood pulp fibre forms, wherein nanometer ZrO 2Complex polyester functional fibre content is not less than 25wt%.
9. the described nanometer ZrO of claim 1 2Complex polyester functional fibre application process; It is characterized in that: that adopts that part or all of this fiber can be made into has emitting biological infrared waves, a uvioresistant, is used to keep healthy, CRUX dress ornament, underwear, bedding, shirt, socks and the various protector goods of sun-proof, insulation.
CN2012101734554A 2012-05-31 2012-05-31 Nano ZrO2 composite polyester functional fiber, manufacturing method thereof and application Pending CN102660799A (en)

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CN108728983A (en) * 2018-05-31 2018-11-02 江苏康溢臣生命科技有限公司 A kind of fabric and its weaving process with zirconium base shield
CN109112663A (en) * 2018-08-16 2019-01-01 王泉泉 It is a kind of to utilize organic carboxyl acid barium salt preparation adjustable polyester fiber of high light transmission refractive index and preparation method thereof
CN109505026A (en) * 2018-12-27 2019-03-22 江苏恒力化纤股份有限公司 Moisture absorption sweat-releasing terylene fiber and preparation method thereof
CN112553734A (en) * 2020-11-30 2021-03-26 闽江学院 Method for preparing non-ironing multifunctional blended yarn by utilizing electrostatic spinning nanotechnology
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CN105088389A (en) * 2015-08-17 2015-11-25 俞尧芳 Anti-ultraviolet polyester fibers and preparation method thereof
CN107987317A (en) * 2017-12-22 2018-05-04 北京化工大学 A kind of preparation method of uvioresistant powder, master batch and PET uvioresistant function fibers
CN108728983A (en) * 2018-05-31 2018-11-02 江苏康溢臣生命科技有限公司 A kind of fabric and its weaving process with zirconium base shield
CN109112663A (en) * 2018-08-16 2019-01-01 王泉泉 It is a kind of to utilize organic carboxyl acid barium salt preparation adjustable polyester fiber of high light transmission refractive index and preparation method thereof
CN109112663B (en) * 2018-08-16 2021-06-15 上海环谷新材料科技发展有限公司 High-light-transmittance and adjustable-refractive-index polyester fiber prepared from organic barium carboxylate and preparation method thereof
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CN109505026B (en) * 2018-12-27 2020-10-16 江苏恒力化纤股份有限公司 Moisture-absorbing sweat-releasing polyester fiber and preparation method thereof
CN112553734A (en) * 2020-11-30 2021-03-26 闽江学院 Method for preparing non-ironing multifunctional blended yarn by utilizing electrostatic spinning nanotechnology
EP4083281A1 (en) * 2021-04-15 2022-11-02 Taiwan Textile Research Institute Temperature-sensing and humidity-controlling fiber and fabricating method thereof

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