CN101573481A

CN101573481A - Nonwovens fabrics produced from multicomponent fibers comprising sulfopolyesters

Info

Publication number: CN101573481A
Application number: CNA2007800491694A
Authority: CN
Inventors: R·K·古普塔; D·W·克罗西维奇; S·E·乔治
Original assignee: Eastman Chemical Co
Current assignee: Eastman Chemical Co
Priority date: 2007-01-03
Filing date: 2007-12-17
Publication date: 2009-11-04
Also published as: KR20090096620A; EP2099962A2; WO2008085332A3; TW200840895A; WO2008085332A2; US20080160859A1; JP2010514957A

Abstract

The present invention provides a process for making a nonwoven fabric comprising: (A) collecting multicomponent fibers to form a non-woven web; wherein the multicomponent fiber comprises at least one water dispersible sulfopolyester and at least one water non-dispersible polymer; wherein said multicomponent fiber has a plurality of domains comprising the water non-dispersible polymer; wherein the domains are substantially isolated from each other by the water dispersible sulfopolyester intervening between the domains; (B) contacting the non-woven web with water at a sufficient temperature and pressure to remove a portion of the water dispersible sulfopolyester thereby forming a microfiber web; and (C) hydroentangling the microfiber web to produce the nonwoven fabric. A process is also provided wherein steps (B) and (C) are combined. Fibrous articles utilizing the nonwoven fabrics are also provided.

Description

Supatex fabric by the multicomponent fibre production that comprises sulfonic polyester

Technical field

The present invention relates to be used for being produced by multicomponent fibre the method for supatex fabric, wherein multicomponent fibre comprises the polymer that dispersible sulfonic polyester of at least a water and at least a water can not disperse.

Background technology

Conventional fabric is by woven or knitting the manufacturing.Supatex fabric is similar to woven and knit goods part and is that the both is loose structure plane, intrinsic flexibility, that be made of polymer-based material.Both main distinctions are to make the method for fabric.Woven fabric is to make two or organize yarn more and make each other in weave in squarely by the order with defined.Supatex fabric is by with the fiber of predetermined number or long filament places two-dimensional array and they are locked together make.Supatex fabric can be interlocked the layer of fiber, long filament or yarn or network by machinery, chemistry or heat mode and be assembled.Typically, the method that is used to produce supatex fabric can be divided into four big classes: textiles, paper is extruded and is mixed (being meant the combination of these technology of use).These fabrics are structures of technical somewhat complex design, and it can be made into and similar in appearance to woven fabric and can surpass the performance of woven fabric.

That extruding technology is used to produce is spunbond, melt and spray and the porous membrane non-weaving cloth.This class non-weaving cloth is become the non-weaving cloth of polymer-laying sometimes.Spunbond and meltblowing method is improving one's methods in the supatex fabric production, because non-weaving cloth is directly made from making the used material of fiber itself, has eliminated the fiber production step thus.Spunbond method directly shifts polymer (tranforms) in the following manner to fabric: extrude long filament, with its orientation bunchy or bunch, its shop layer is interlocked it carrying on the screen cloth and by the combination of heat fusion, mechanical interlocking, chemical adhesion or these methods.In meltblowing method, polymer be heated to liquid state and when its when the extrusion cavities, its in about 250 to 500 ℃ of injections with velocity of sound air.The air logistics of fast moving stretches molten polymer and it is solidified to produce fine fibre.Fiber separates with the air logistics with the form of entangled web then and pushes between warm-up mill.

In textile application (clothes, curtain, upholstery and uniform), use non-weaving cloth.Supatex fabric can also be used for the personal care product, as but be not limited to rag, feminine hygiene, baby diaper, adult-incontinence underpants and hospital/surgery and other medical disposable product.Other is used including, but not limited to protection fabric and layer, geotextile, industrial wipes and filter medium.

Therefore, need to produce the new method of supatex fabric and fibre prepared therefrom, it is more effective and/or more cheap.The invention provides new method by the multicomponent fibre production supatex fabric that comprises the polymer that dispersible sulfonic polyester of at least a water and at least a water can not disperse.

Summary of the invention

In one embodiment of the present invention, provide a kind of method of making supatex fabric.This method comprises: (A) collect multicomponent fibre to form nonwoven web; Wherein multicomponent fibre comprises the polymer that dispersible sulfonic polyester of at least a water and at least a water can not disperse; Wherein multicomponent fibre has a plurality of territories, and described territory comprises the polymer that water can not disperse; Wherein said territory is isolated from each other basically by the dispersible sulfonic polyester of the water between described territory; (B) nonwoven web is contacted with water and remove a part the dispersible sulfonic polyester of water, form microfiber webs thus; (C) water tangles (hydroentangling) microfiber webs to produce supatex fabric.

In another embodiment of the present invention, provide the method for another kind of manufacturing supatex fabric.This method comprises: (A) collect multicomponent fibre to form nonwoven web; Wherein multicomponent fibre comprises the polymer that dispersible sulfonic polyester of at least a water and at least a water can not disperse; Wherein multicomponent fibre has a plurality of territories, and described territory comprises the polymer that water can not disperse; Wherein said territory is isolated from each other basically by the dispersible sulfonic polyester of the water between described territory; (B) nonwoven web is contacted with water and remove the dispersible sulfonic polyester of water of a part, form microfiber thus, and the microfiber of water entanglement simultaneously is to produce supatex fabric.

Our invention provides method new and cheap production supatex fabric thus.Supatex fabric can be the form of open width fabric (flat fabric) or 3D shape and can be incorporated into various fibres as the aforementioned in those.

Description of drawings

Fig. 1 for example understands spunbond method.

Fig. 2 illustrates embodiment and how to be relative to each other.

The specific embodiment

By the following detailed description of preferred embodiments of reference the present invention and the embodiment that is comprised herein and with reference to the accompanying drawings and explanation previous and subsequently, the present invention can be easier to obtain understand.

Before disclosure and description The compounds of this invention, composition, goods, equipment and/or method, be to be understood that the present invention is not limited to concrete synthetic method, concrete technology or concrete device, it certainly changes.Should be appreciated that equally term used herein only is in order to describe the purpose of specific embodiments, to be not intended to be used to limit.

In this specification and claim subsequently, somely should be defined as term with following implication with mentioning.

Unless clearly demonstrate in addition in context, the singulative that uses in specification and appended claims " a ", " an " and " the " comprise that plural number mentions thing.Thus, for example, polymer comprises one or more (kind) polymer.

In this article, scope can be expressed as from " pact " specific value, and/or to " pact " another specific value.When being expressed as described scope, another embodiment comprises since an occurrence and/or to another occurrence.Similarly, when " pact " by priority of use is approximation with numeric representation, be to be understood that this specific value has formed another embodiment.The end points that should be appreciated that each scope in addition is with respect to other end points with to be independent of all be important aspect two outside other end points.Further, in the scope described in this specification and claim intention particularly including gamut, but not end points only.For example, be described as 0～10 scope intention and disclose all integers between 0～10, such as 1,2,3,4 etc., all marks between 0～10, for example 1.5,2.3,4.57,6.1113 etc., and end points 0 and 10.And, the scope relevant with chemical substituted radical, for example " C1-C5 hydro carbons " is intended to comprise especially and disclose C1 and C5 hydro carbons and C2, C3 and C4 hydro carbons.

" optional " or " randomly " is meant that incident or the situation described subsequently may exist or may not exist, and described description comprises situation and wherein said incident or the non-existent situation of environment that wherein said incident or environment exist.For example, phrase " optional heat " is meant that this material may be heated or may not be heated, and this phrase comprises process heating and that do not have heating.

Unless otherwise stated, all numerals of quantity, performance such as molecular weight, the reaction condition etc. of used expression composition should be understood that in all instances " pact " modifies by term in specification and the claim.Therefore, unless point out on the contrary, be similar at the numerical parameter described in following specification and the claims, it can change, and this depends on the performance of managing by the expectation of the present invention's acquisition.At least, each numerical parameter should be understood according to the number of the significant digits of being reported and by using the conventional technology of rounding at least.Although number range and parameter listed in broad range of the present invention all are approximations, the numerical value of listing in the specific embodiment is all as far as possible accurately reported.Yet any numerical value all comprises some error that must come from its standard deviation that exists in thermometrically separately inherently.

As used in this article, term " supatex fabric " or " nonwoven web " are meant that a kind of is not to insert the middle single fiber or the structure of line in discernible mode (as in the knitted fabric).Basis weight of nonwoven fabrics is typically expressed as the ounce every square yard (osy) of material or restrains every square metre (gsm).

As used in this article, term " fiber " is meant the extrudate by the elongation that polymer is formed by shaped hole such as die head.Unless otherwise noted, term " fiber " comprises the strand and continuous material strand at intermittence with definite length, as long filament.Supatex fabric of the present invention can be formed by multicomponent cut staple (staple multicomponent fiber).Such cut staple can be by combing and bonding and form supatex fabric.Yet, making us desirably, supatex fabric of the present invention is to use continuous multicomponent filaments to make, and it is extruded, and stretches and is laid on the mobile profiled surface.

As used in this article, term " microfiber " is meant small diameter fibers, and its average diameter is not more than about 12 microns, and for example average diameter is about 3 microns-Yue 8 microns.Fiber is also described with the dawn number usually.Less dawn numerical table shows more tiny fiber, and higher dawn numerical table shows thicker or bigger fiber.For example, the dawn number of 15 microns polypropylene fibres is about 1.42 (15 ²* 0.89 * 0.00707=1.415).Be used to produce the employed microfiber of supatex fabric of the present invention and typically have following d/f value: 1 or littler, 0.5 or littler, or 0.1 or littler.

As used in this article, term " multicomponent fibre " or " conjugate fibre " are meant such fiber, and it is formed by at least two kinds of polymers compositionss.Such fiber is extruded from independent extruder usually, but spinning forms a fiber together.The polymer of respective components differs from one another usually, yet multicomponent fibre can comprise the independent component of similar or identical polymeric material.Independent component is typically arranged in different sections (segment) that fixedly install basically or district and is extended along the whole length of multicomponent fibre basically along the section of multicomponent fibre.The configuration of such multicomponent fibre can for example be parallel type structure, cake type (pie) structure or other structure.Multicomponent fibre has obtained instruction: U.S.Pat.No.5,108,820 (Kaneko etc.) with the method for making it in following document; U.S.Pat.No.4,795,668 (Krueger etc.); U.S.Pat.No.5,382,400 (Pike etc.); U.S.Pat.No.5,336,552 (Strack etc.); U.S. patent application Ser.No.08/550,042 (October 30 1996 applying date, Cook); With U.S. patent application Ser.No.11/344,320 (on January 31st, 2006, Gupta etc.).Fiber and comprise that its independent component also can have various irregular shapes, those described in following document: U.S.Pat.No.5,277,976 (Hogle etc.); U.S.Pat.Nos.5,162,074 and 5,466,410 (Hills); And U.S.Pat.Nos.5,069,970 and 5,057,368 (Largman etc.). the full content of above-mentioned patent and application under its degree of not runing counter to statement herein, is incorporated herein by reference.

As used in this article, term " polymer " " generally include but be not limited to homopolymers, copolymer, for example block, grafting, random and alternate copolymer, trimer etc. and its blend and modifier.In addition, unless in addition special restriction, term " polymer " " should comprise the whole possible geometric configuration of molecule.These configurations are including, but not limited to isotaxy, syndiotactic and atactic symmetries.

As used in this article, about the dispersible sulfonic polyester of water as a kind of component of multicomponent fibre, term " water is dispersible " intention and term " water-can disperse ", " water-separable ", " water-soluble ", " water is eliminable ", " water miscible ", " water-removable ", " water-soluble " and " water dispersible " synonym, and intention is meant that the sulfonic polyester component is removed fully and dispersed or dissolved under the effect of water from multicomponent fibre, thereby can discharge and separate the polymer fiber that wherein contained water can not disperse.Term " dispersion ", " dispersible ", " dispersing " or " can disperse " are meant, the deionized water of use q.s (for example, 100: 1 water: fiber, by weight) to form the loose suspension or the slurry of fiber, under about 60 ℃ temperature, with in time of 5 days at the most, the sulfonic polyester component with the multicomponent fibre dissolving, decompose or separate with it, from the polymer section (segment) that water can not disperse, stay a plurality of microfibers.Within the scope of the invention, all these terms mixture of being meant water or water and water-mixable cosolvent to the activity of the dispersible sulfonic polyester of described water herein.The example of this water-mixable cosolvent is including, but not limited to alcohol, ketone, glycol ethers (glycol ethers), ester or the like.For this term, intention comprises such situation, and wherein the dispersible sulfonic polyester of water is dissolved forming true solution, and wherein the dispersible sulfonic polyester of water is dispersed in the aqueous medium those.Usually, because the statistics character of sulfonic polyester composition when single sulfonic polyester sample is placed aqueous medium, might have soluble fraction and dispersed fraction.

Term " section (segment) " or " territory " or " district ", when being used to describe the shaping section of multicomponent fibre, be meant the zone in the section of the polymer that comprises that water can not disperse, wherein these territories or section (segment) are isolated from each other basically by the dispersible sulfonic polyester of water between section (segment) or territory.As used in this article, term " substantial barrier ", intention is meant that section (segment) or territory are separated from each other, thereby when removing sulfonic polyester, allows section (segment), territory to form independent fiber.Section (segment) or territory or district can have similar size and shape or different size and shapes.In addition, section (segment) or territory or district can arrange with any configuration.These sections (segment) or territory or district are " continuous basically " along the length direction of multicomponent extrudate or fiber.Term " continuous basically " is meant that along at least 10 centimetres length of multicomponent fibre be continuous.

The invention provides the method for producing supatex fabric from multicomponent fibre, wherein multicomponent fibre comprises the polymer that dispersible sulfonic polyester of at least a water and at least a water can not disperse.

In one embodiment, provide a kind of method, it comprises: (A) collect multicomponent fibre to form nonwoven web; Wherein multicomponent fibre comprises the polymer that dispersible sulfonic polyester of at least a water and at least a water can not disperse; Wherein multicomponent fibre has a plurality of territories, and described territory comprises the polymer that water can not disperse; Wherein said territory is isolated from each other basically by the dispersible sulfonic polyester of the water between described territory; (B) nonwoven web is contacted with water and remove a part the dispersible sulfonic polyester of water, form microfiber webs thus; (C) water entanglement microfiber webs is to produce supatex fabric.

The blend of the polymer that the multicomponent fibre of our invention can not disperse by the single sulfonic polyester of melt-spun or sulfonic polyester with the immiscible water of sulfonic polyester prepares.For example at United States Patent (USP) 5,916, in 678, by extruding the polymer that sulfonic polyester and one or more water can not disperse, the latter is immiscible with sulfonic polyester, (for example, fabric of island-in-sea type, core-skin type, parallel type or fan cake type (segmented pie) configuration) spinnerets has prepared a kind of multicomponent fibre by having shaping or processing cross-section geometry individually.By dissolving boundary layer or pie section (segment) and stay the less long filament of the polymer that water can not disperse or microfiber and remove the dispersible sulfonic polyester that anhydrates subsequently.The fiber size that these fibers of the polymer that water can not disperse have is far smaller than the size of the multicomponent fibre before removing the dispersible sulfonic polyester that anhydrates.

In one embodiment, multicomponent fibre is by following manner production: the polymer feed that sulfonic polyester and water can not be disperseed is to the polymer distribution system, and wherein polymer is introduced into fan-shaped (segmented) spinnerets.Polymer arrives fiber spinneret according to independent path, and in the combination of spinneret hole place, described spinneret hole comprises two concentric circular holes, thereby provide sheath core fiber, perhaps it comprises circular spinneret hole, this spinneret hole is divided into a plurality of parts along diameter, thereby bilateral fibre is provided.Perhaps, dispersible sulfonic polyester of immiscible water and the water polymer that can not disperse can be introduced the spinnerets with a plurality of radial passages has fan cake type (segmented pie) section with production multicomponent fibre individually.Usually, sulfonic polyester will form core-skin type configuration " skin " component.In the fiber section with a plurality of sections (segment), the section that water can not disperse (segment) usually, is isolated from each other basically by sulfonic polyester.

Perhaps, multicomponent fibre can form like this, be included in the polymer that fusion sulfonic polyester and water can not disperse in the independent extruder, and polymer flow is imported the spinnerets with a plurality of distribution flow paths, and form is that little tubule or section (segment) are to provide the multicomponent fibre with fabric of island-in-sea type shaping section.The case description of this spinnerets is at United States Patent (USP) 5,366, in 804, under its degree of not runing counter to statement herein, is incorporated herein by reference.In the present invention, usually, sulfonic polyester will form " sea " component, and the polymer that water can not disperse will form " island " component.

As illustrated among the present invention, the shaping section of multicomponent fibre can for example be following form: core-skin type, fabric of island-in-sea type, fan cake type (segmented pie), hollow fan cake type (hollowsegmented pie), eccentric fan cake type (off-centered segmented pie) or the like.

Multicomponent fibre of the present invention is by polyester, perhaps more particularly, and sulfonic polyester, preparation, it comprises dicarboxylic acid monomer's residue, sulfomonomer residue, diol monomer residue and repetitive.Sulfomonomer can be dicarboxylic acids, glycol or hydroxycarboxylic acid.Therefore, term " monomer residue " as used in this article, is meant the residue of dicarboxylic acids, glycol or hydroxycarboxylic acid." repetitive " as used in this article, is meant to have 2 organic structures by the monomer residue of carbonyl oxygen base connection.Sulfonic polyester of the present invention comprises the sour residue (100mol%) and the glycol residue (100mol%) of first-class substantially mol ratio, and its ratio reaction to equate basically makes the total mole number of repetitive equal 100mol%.Therefore, the molar percentage that provides in the present disclosure can be based on the total mole number of sour residue, the total mole number of glycol residue or the total mole number of repetitive.For example, what comprise 30mol% based on total repetition unit can be that the sulfonic polyester of the sulfomonomer of dicarboxylic acids, glycol or hydroxycarboxylic acid is meant such sulfonic polyester, in the repetitive of 100mol% altogether, comprises the 30mol% sulfomonomer.Therefore, in every 100mol repetitive, there is the sulfomonomer residue of 30mol.Equally, comprise the sulfonic polyester of the dicarboxylic acids sulfomonomer of 30mol%, be meant that sulfonic polyester comprises the 30mol% sulfomonomer in 100mol% acid residue altogether based on the total acid residue.Therefore, in one situation of back, in per 100 moles sour residue, there is the sulfomonomer residue of 30mol.

Described herein sulfonic polyester has the logarithmic viscosity number at least about 0.1dL/g, be abbreviated as " Ih.V. " hereinafter, at the measurement of concetration of 25 ℃ of sulfonic polyesters of about 0.5g in the solution of the phenol/tetrachloroethane solvent of 60/40 weight portion and in the solvent of 100mL.The logarithmic viscosity number of sulfonic polyester can be about 0.2-0.3dl/g.Another scope of logarithmic viscosity number is greater than about 0.3dl/g.As used in this article, term " polyester " comprises " all polyester " and " copolyesters " and is meant the synthetic polymer that the polycondensation by bifunctional carboxylic acid and difunctionality hydroxy compounds prepares.As used in this article, term " sulfonic polyester " meaning is any polyester that comprises sulfomonomer.

Usually the bifunctional carboxylic acid is a dicarboxylic acids, and the difunctionality hydroxy compounds is a dihydroxylic alcohols, for example glycol (glycol) and glycol (diol).Perhaps, the bifunctional carboxylic acid is a hydroxycarboxylic acid, P-hydroxybenzoic acid for example, and the difunctionality hydroxy compounds may be the aryl nucleus that has 2 hydroxyl substituents, for example quinhydrones.As used in this article, term " residue " meaning is any organic structure of introducing polymer by the polycondensation reaction that relates to corresponding monomer.Therefore, the dicarboxylic acids residue can be derived from dicarboxylic acid monomer or its relevant carboxylic acid halides, ester, salt, acid anhydrides or its mixture.Therefore, as used in this article, term dicarboxylic acids intention comprises any derivative of dicarboxylic acids and dicarboxylic acids, comprises carboxylic acid halides, ester, half ester, salt, half salt, acid anhydrides, mixed acid anhydride or its mixture that it is relevant, and they can be used for polycondensation process with glycol with the preparation high molecular weight polyesters.

Sulfonic polyester of the present invention comprises one or more dicarboxylic acids residues.The type and the concentration that depend on sulfomonomer, dicarboxylic acids residue can comprise the sour residue of the about 100 moles of % of about 60-.Other examples of the concentration range of dicarboxylic acids residue are about 95 moles of % of about 60 moles of %-and the about 95 moles of % of about 70 moles of %-.The example of operable dicarboxylic acids comprises aliphatic dicarboxylic acid, alicyclic dicarboxylic acid, aromatic dicarboxylic acid, or two or more these sour mixture.Therefore, suitable dicarboxylic acids is including, but not limited to, butanedioic acid; Glutaric acid; Adipic acid; Azelaic acid; Decanedioic acid; Fumaric acid; Maleic acid; Itaconic acid; 1, the 3-cyclohexane dicarboxylic acid; 1, the 4-cyclohexane dicarboxylic acid; Diglycolic acid; 2,5-norcamphane dicarboxylic acids; Phthalic acid; Terephthalic acid (TPA); 1, the 4-naphthalene dicarboxylic acids; 2, the 5-naphthalene dicarboxylic acids; Diphenic acid; 4,4 '-oxydiphenyl formic acid (oxydibenzoic); 4,4 '-sulfonyldibenzoic acid; And M-phthalic acid.Preferred dicarboxylic acids residue is M-phthalic acid, terephthalic acid (TPA) and 1, and the 4-cyclohexane dicarboxylic acid is if perhaps use diester, dimethyl terephthalate (DMT), dimethyl isophthalate and 1,4-cyclohexane dicarboxylic acid dimethyl ester.Although the dicarboxylic acids methyl esters can be used, also acceptable is the ester that comprises high-order (higher order) alkyl, for example ethyl, propyl group, isopropyl, butyl or the like.In addition, aromatic ester, particularly phenylester also can use.

Sulfonic polyester comprises the about 40mol% of about 4-, based on total repetition unit, the residue of at least a sulfomonomer, one or more sulfonate groups that it has 2 functional groups and is attached to aromatics or cyclic aliphatic ring, wherein this functional group is a hydroxyl, carboxyl or its combination.Other example for the concentration range of sulfomonomer residue is the about 35 moles of % of about 4-, and the about 25 moles of % of the about 30 moles of % of about 8-and about 8-are based on total repetitive.Sulfomonomer can be the dicarboxylic acids or its ester that comprise sulfonate groups, comprise the glycol of sulfonate groups or comprise the hydroxy acid of sulfonate groups.Term " sulfonate " refers to the have structure sulfonate of " SO3M ", and wherein M is the CATION of sulfonate.The CATION of sulfonate can be a metal ion, as Li ⁺, Na ⁺, K ⁺, Mg ⁺⁺, Ca ⁺⁺, Ni ⁺⁺, Fe ⁺⁺Or the like.Perhaps, the CATION of sulfonate can be nonmetal, as, for example, United States Patent (USP) 4,304, the nitrogenous base of describing in 901.The cation source of nitrogen base is in nitrogenous base, and it can be the compound of aliphatic, cyclic aliphatic or aromatics.The example of such nitrogenous base comprises ammonia, dimethylethanolamine, diethanol amine, triethanolamine, pyridine, morpholine and piperidines.Because comprising the monomer of the sulfonate of nitrogen base, to prepare under the condition of polymer of molten condition at needs usually be heat-labile, therefore the method that is used for preparing the sulfonic polyester of nitrogenous basic sulfonate groups of the present invention be with the form of its alkali metal salt will comprise the sulfonate groups of aequum polymer dispersed, disperse or be dissolved in water, use nitrogen base cation exchange alkali metal cation then.

When the monoacidic base metal ion is used as the CATION of sulfonate, resulting sulfonic polyester fully can be dispersed in the water, and the speed of its dispersion (rate) depends on the content of the sulfomonomer in the polymer, the temperature of water, surface area/thickness of sulfonic polyester or the like.When using bivalent metal ion, resulting sulfonic polyester is not easy to be disperseed by cold water, but more easily disperses by hot water.In single polymer composition, utilize greater than a kind of equilibrium ion and be feasible and can provide customization or the method for the water-responsive (water-responsivity) of adjustment resulting product.The example of sulfomonomer residue comprises such monomer residue, and wherein sulfonate groups is connected to aromatic acid ring (nucleus), for example, and benzene; Naphthalene; Phenylbenzene (diphenyl); Oxydiphenyl (oxydiphenyl); Sulphonyl phenylbenzene (sulfonyldiphenyl); With methylene phenylbenzene (methylenediphenyl), or the cyclic aliphatic ring, for example, cyclohexyl; Cyclopentyl; Cyclobutyl; Suberyl and ring octyl group.Other example that can be used for sulfomonomer residue of the present invention is the metal sulfonate of sulfosalicylic phthalate, sulfo group terephthalic acid (TPA), sulfoisophthalic acid or its combination.Other example of operable sulfomonomer is that 5-sodium is for sulfoisophthalic acid and its ester.If for sulfoisophthalic acid, the sulfomonomer concentration range is the about 35 moles of % of about 4-to the sulfomonomer residue usually from 5-sodium, the about 30 moles of % of about 8-and about 8-25 mole % are based on the total mole number of sour residue.

The sulfomonomer that is used in the preparation sulfonic polyester is compound known and can uses method preparation well-known in the art.For example, wherein the sulfonate groups sulfomonomer that is connected to aromatic ring can prepare like this, comprise with fuming sulphuric acid sulfonated aromatic compound to obtain corresponding sulfonic acid, and then with metal oxide or alkali, for example, and sodium acetate, reaction prepares sulfonate.The method for preparing different sulfomonomers is described in, for example, and United States Patent (USP) 3,779,993; In 3,018,272 and 3,528,947.

Also possible is when polymer is the form of disperseing, use, for example, sodium sulfonate, with ion-exchange process come with as the different ion replacement sodium of zinc etc. prepare polyester.In the usually easier scope that is dissolved in polymer reaction thing fusion phase of sodium salt, such ion-exchange process is better than preparing polymer with divalent salts usually.

Sulfonic polyester comprises one or more glycol residues, and it can comprise aliphatic series, cyclic aliphatic and aralkyl glycol.Cycloaliphatic diol, for example, 1,3-and 1,4 cyclohexane dimethanol, may with they the pure cis or the form of transisomer or exist with the form of cis and transisomer mixture.As used in this article, term " glycol (diol) " and term " glycol (glycol) " synonym, and be meant any dihydroxylic alcohols.The example of glycol includes, but are not limited to, ethylene glycol; Diethylene glycol (DEG); Triethylene glycol; Polyethylene glycol; 1, ammediol; 2,4-dimethyl-2-ethyl hexane-1,3-glycol; 2,2-dimethyl-1, ammediol; 2-ethyl-2-butyl-1, ammediol; 2-ethyl-2-isobutyl group-1, ammediol; 1,3 butylene glycol; 1, the 4-butanediol; 1, the 5-pentanediol; 1, the 6-hexylene glycol; 2,2,4-trimethyl-1,6-hexylene glycol; Thiodiethanol; 1, the 2-cyclohexanedimethanol; 1, the 3-cyclohexanedimethanol; 1,4 cyclohexane dimethanol; 2,2,4,4-tetramethyl-1,3-cyclobutanediol; Terephthalyl alcohol (xylylenediol), or one or more the combination in these glycol.

The glycol residue can comprise the about 100 moles of % of about 25 moles of %-, based on the total diol residue, the residue of poly-(ethylene glycol) with following structure

H-(OCH ₂-CH ₂) _n-OH

Wherein n is the integer of 2-about 500.The limiting examples of the polyethylene glycol of lower molecular weight, for example, wherein n is 2-6, is diethylene glycol (DEG), triethylene glycol and tetraethylene glycol.In the glycol of these lower molecular weights, diethylene glycol (DEG) and triethylene glycol are preferred.The polyethylene glycol of higher molecular weight (being abbreviated as " PEG " at this), wherein n is that 7-is about 500, comprises that the commercially available known name that gets is called

Product, it is the product of Dow Chemical Company (UnionCarbide in the past).Usually, PEG and other diol combination are used, and described glycol for example is diethylene glycol (DEG) or ethylene glycol.Based on the value of n, it changes in greater than 6 to 500 scopes, and molecular weight can change between the 000g/mol about 22 greater than 300-.Molecular weight and mole % are each other in inverse ratio; Specifically, along with the increase of molecular weight, mole % will reduce to reach the hydrophily of given extent.For example, this conceptual illustration be PEG that imagination has 1000 molecular weight can constitute total diol up to 10 moles of %, will be usually introduce and have the PEG of 10,000 molecular weight with the level of 1 mole of % being lower than total diol.

Because side reaction may form some dimer, trimer and tetramer in position, described side reaction can be controlled by changing process conditions.For example, the diethylene glycol (DEG) of variable quantity, triethylene glycol and tetraethylene glycol can be formed by ethylene glycol, and this comes from incidental acid-catalyzed dehydration reaction when carrying out polycondensation reaction under acid condition.Those skilled in the art are well-known, and the cushioning liquid of existence can add reactant mixture to and postpone these side reactions.But other compositing range is possible, if omit cushioning liquid and allow that dimerization reaction, trimerization reaction and four gather reaction and carry out.

Sulfonic polyester of the present invention can comprise the about 25mol% of 0-, based on total repetition unit, have 3 or the residue of the branched monomer of above functional group, wherein this functional group is a hydroxyl, carboxyl or its combination.The limiting examples of branched monomer is 1,1,1-trimethylolpropane, 1,1,1-trimethylolethane, glycerine, pentaerythrite, erythrite, threitol, dipentaerythritol, D-sorbite, trimellitic anhydride, pyromellitic acid dianhydride, dihydromethyl propionic acid or its combination.The further example of branched monomer concentration range is about 20mol% of 0-and the about 10mol% of 0-.The existence of branched monomer may cause the many possible benefit to sulfonic polyester of the present invention, includes but not limited to, to the ability of custom stream sex change, dissolubility and tensile property.For example, under constant molecular weight, the sulfonic polyester of branching is compared with the analog of linearity, will have bigger ends concentration, and it can promote cross-linking reaction after the polymerization.But under high branching agent concentration, sulfonic polyester may be inclined to gelation.

Be used for the glass transition temperature that the sulfonic polyester of multicomponent fibre of the present invention has, be abbreviated as " Tg " at this, be at least 25 ℃, its standard technique that is to use differential scanning calorimetry (" DSC ") as well known to the skilled person is to the polymer measurement of drying.The Tg measurement of sulfonic polyester of the present invention is to use " dry polymer " to carry out, that is, a kind of polymer samples wherein disperses water external or that absorb by polymer being heated to about 200 ℃ temperature and making sample get back to room temperature.Usually, sulfonic polyester in the DSC instrument by carrying out initial heat scan drying, wherein, sample is heated to the temperature greater than the water vapor temperature, sample remain on the water that in polymer, absorbs under this temperature vaporize fully till (as indicated) by big, wide heat absorption, the sample cool to room temperature, carry out second time heat scan then and measure to obtain Tg.The further example of the glass transition temperature that sulfonic polyester demonstrates is at least 30 ℃, at least 35 ℃, and at least 40 ℃, at least 50 ℃, at least 60 ℃, at least 65 ℃, at least 80 ℃ and at least 90 ℃.Although other glass transition temperature is possible, in our invention, the common glass transition temperature of dry sulfonic polyester is about 30 ℃, about 48 ℃, and about 55 ℃, about 65 ℃, about 70 ℃, about 75 ℃, about 85 ℃ and about 90 ℃.

In another embodiment, yet sulfonic polyester of the present invention can be single polyester, perhaps, can change the performance of the multicomponent fibre of gained with one or more auxiliary polyblends.Auxiliary polymer can be or can not be that water is dispersible that this depends on application, and can be mixable or immiscible with sulfonic polyester.If auxiliary polymer is that water can not disperse, the blend that preferably has sulfonic polyester is immiscible.Term " mixable ", as used in this article, intention is meant that blend has amorphous phase single, homogeneous, as specified by the Tg of single composition-rely on.For example, can be used for " plasticising " second polymer with mixable first polymer of second polymer, for example, as at United States Patent (USP) 6,211, institute is illustrational in 309.By contrast, term " immiscible " as used in this article, is represented such blend, and it demonstrates at least 2, the phase of mixing at random and demonstrates more than a Tg.Some polymer can be immiscible with sulfonic polyester, but compatible with sulfonic polyester.The further general introduction of mixable and immiscible blend polymer and the various analytical technologies that are used for its sign are found in following document: Polymer Blends (blend polymer) volume 1 and 2, editor D.R.Paul and C.B.Bucknall, 2000, John Wiley ﹠amp; Sons, Inc.

Can be polymethylacrylic acid with the limiting examples of the water dispersible polymers of sulfonic polyester blend, PVP, polyethylene-acrylic copolymer, polyvinyl methyl ether, polyvinyl alcohol, polyethylene glycol oxide, hydroxy propyl cellulose, hydroxypropyl methylcellulose, methylcellulose, ethylhydroxyethylcellulose, the isopropyl cellulose, methyl ether starch, polyacrylamide, poly-(N-caprolactam), the Ju ethyl oxazoline, poly-(2-isopropyl-2-oxazoline), Ju vinyl methyl oxazolidinone, the dispersible sulfonic polyester of water, Ju vinyl methyl oxazolidinone (oxazolidimone), poly-(2,4-dimethyl-6-triazine radical ethene) and ethylene oxide-propylene oxide copolymer.The example of the polymer that can not disperse with the water of sulfonic polyester blend is including, but not limited to the polyene footpath, as polyethylene and polyacrylic homopolymers and copolymer; Poly-(Polyethyleneglycol Terephthalate); Poly-(butylene terephthalate); And polyamide, as nylon-6; Polyactide; Caprolactone; Eastar

(poly-(tetramethylene adipate ester-co-terephthalate), the product of Eastman ChemicalCompany); Merlon; Polyurethane; And polyvinyl chloride.

According to our invention, can be used to customize gained supatex fabric or fibroreticulate terminal serviceability more than a kind of blend of sulfonic polyester.The blend of one or more sulfonic polyesters will have at least 25 ℃ glass transition temperature.Therefore, thereby also can being utilized, blend changes the manufacturing of the processing characteristics promotion supatex fabric of sulfonic polyester.

Sulfonic polyester and auxiliary polymer can with intermittently, semicontinuous or continuous process carries out blend.Small-scale batch of material can be easy to be prepared in the well-known any high-intensity mixing device of those skilled in the art, as Banbury mixer, and melt-spun fibre then.Described component also can be carried out blend in solution in suitable solvent.Melt-mixing method is included in blend sulfonic polyester and auxiliary polymer under the temperature that is enough to molten polymer.Blend can be cooled and granulation so that further use, perhaps melt blended material can directly be melt-spun into fibers form by this melt blended material.Term " fusion ", as used in this article, including, but not limited to only softening polyester.For common known melting mixing method in the technical field of polymer, referring to Mixing and Compounding of Polymers (I.Manas-Zloczower ﹠amp; Z.Tadmoreditors, Carl Hanser Verlag Publisher, 1994, New York, N.Y.).

In another embodiment of the present invention, the glass transition temperature of the sulfonic polyester in the multicomponent fibre (Tg) is at least 25 ℃, and this sulfonic polyester comprises:

(A) one or more residues of the M-phthalic acid of the about 96mol% of about 50-or terephthalic acid (TPA) are based on the total acid residue;

(B) the about 30mol% of about 4-, based on the total acid residue, sodium for the residue of sulfoisophthalic acid;

(C) one or more glycol residues, wherein 25mol% at least based on the total diol residue, is poly-(ethylene glycol) with following structure

H-(OCH ₂-CH ₂) _n-OH

Wherein n is the integer of 2-about 500; The (iv) about 20mol% of 0-, based on total repetition unit, have 3 or the residue of the branched monomer of above functional group, wherein this functional group is a hydroxyl, carboxyl or its combination.

As noted before, multicomponent fibre can randomly comprise the first water dispersible polymers with the sulfonic polyester blend; With, randomly, the polymer with the water of sulfonic polyester blend can not disperse makes that this blend is immiscible blend.The first water dispersible polymers is as described above.Sulfonic polyester can have at least 25 ℃ glass transition temperature (Tg), but can have for example following Tg: about 35 ℃, about 48 ℃, about 55 ℃, about 65 ℃, about 70 ℃, about 75 ℃, about 85 ℃ and about 90 ℃.Sulfonic polyester can comprise the M-phthalic acid residue of other concentration, for example, and about 95 moles of % of about 60 moles of %-and the about 95 moles of % of about 70 moles of %-.The further example of the concentration range of M-phthalic acid residue is the about 85 moles of % of about 70 moles of %-, about 95 moles of % of about 85 moles of %-and the about 95 moles of % of about 90 moles of %-.Sulfonic polyester can also comprise the residue of the diethylene glycol (DEG) of the about 95mol% of about 25-.The further example of the concentration range of diethylene glycol (DEG) residue comprises the about 95mol% of about 50-, the about 95mol% of about 70-and the about 95mol% of about 75-.Sulfonic polyester can also comprise the residue of ethylene glycol and/or 1,4 cyclohexane dimethanol (being abbreviated as " CHDM " in this article).The typical concentrations scope of CHDM residue is the about 75mol% of about 10-, the about 65mol% of about 25-and the about 60mol% of about 40-.The typical concentrations scope of ethylene glycol residue is the about 75mol% of about 10-, the about 65mol% of about 25-and the about 60mol% of about 40-.In another embodiment, sulfonic polyester comprises the residue of the diethylene glycol (DEG) of the residue of M-phthalic acid of the about 96mol% of about 75-and the about 95mol% of about 25-.

Sulfonic polyester of the present invention uses typical polycondensation reaction condition, is easy to by suitable dicarboxylic acids, ester, acid anhydrides or salt, and sulfomonomer and suitable glycol or diol mixture prepare.They can prepare and can utilize various type of reactor by mode of operation continuous, semicontinuous and intermittently.The example of suitable type of reactor including, but not limited to agitator tank, continuous stirring jar, slurry phase reactor, tubular reactor, wipe film reactor (wiped-film reactor), falling film reactor or extrusion reaction device.Term " continuously " as used in this article, is meant a kind of method, and wherein the recovery of the introducing of reactant and product is carried out simultaneously with non-discontinuous manner." continuously " is meant that in operation this method is basically or totally continuous, forms contrast with " intermittently " method." continuously " mean never in any form forbid in successional method because for example start, reactor maintenance or be scheduled to the normal interruption that the parking cycle caused.Term " intermittently " method as used in this article, is meant a kind of method, wherein the total overall reaction thing is added in the reactor, handle according to predetermined course of reaction subsequently, during this period, do not have material to be fed in the reactor or from reactor, take out material.Term " semicontinuous " is meant a kind of method, and the some of them reactant adds when method begins, and remaining reactants charging continuously along with the reaction development.Perhaps, semi-continuous process also can comprise a kind of method that is similar to batch process, wherein when method begins, adds whole reactants, and different is along with the reaction development, to take out one or more products continuously.It is favourable that described method is operated in the mode of continuous process, this is for economic reasons, and so that produce the good color of polymer, because if sulfonic polyester is at high temperature stopped the oversize time in reactor, it is possible deviation in appearance.

Sulfonic polyester of the present invention prepares by method known to those skilled in the art.Sulfomonomer is the most directly added in the reactant mixture, prepares polymer by described reactant mixture, but additive method be known and can be used, for example, as United States Patent (USP) 3,018,272,3,075,952 and 3,033, described in 822.Use conventional polyester condition, can carry out sulfomonomer, diol component and dicarboxylic acid component's reaction.

For example, when preparing sulfonic polyester by ester exchange reaction, promptly the ester-formin by the dicarboxylic acid component prepares, and course of reaction can comprise two steps.In first step, diol component and dicarboxylic acid component, for example dimethyl isophthalate is reacted under heating up, and is generally about 150 ℃-Yue 250 ℃, about 8 hours of about 0.5-, pressure be about 0.0kPa (gauge pressure)-Yue 414kPa (gauge pressure) (60 pounds/square inch, " psig ") preferably, the temperature of ester exchange reaction is about 180 ℃-Yue 230 ℃, about 4 hours of about 1-, and preferred pressure for about 103kPa (gauge pressure) (15psig)-Yue 276kPa (gauge pressure) (40psig).

Thereafter, product heats and forms and have the sulfonic polyester of eliminating glycol in higher temperature with at the pressure that reduces, its be under these conditions volatilization easily and from system, be removed.This second step, perhaps condensation polymerization step, under higher vacuum and temperature, continue, be generally about 350 ℃ of about 230 ℃ of .-, preferably about 250 ℃-Yue 310 ℃ and most preferably from about 260 ℃-Yue 290 ℃ reached about 0.1-at about 6 o'clock, perhaps preferably, about 2 hours of about 0.2-is up to the polymer as the degree of polymerization measured according to logarithmic viscosity number that obtains to have expectation.Condensation polymerization step can be carried out at the pressure that reduces, and described pressure is about 53kPa (400 holder)-Yue 0.013kPa (0.1 holder).Stirring or appropriate condition are used in two stages to guarantee the enough heat transmission and the Surface Renewal of reactant mixture.Two stage reaction can be subjected to the promotion of appropriate catalyst, for example, and alkoxy titanium compound, alkali metal hydroxide and alcoholates, the salt of organic carboxyl acid, Alkyzin compound, metal oxide etc.Also can use triphasic manufacture method, be similar to United States Patent (USP) 5,290, those described in 631 particularly when using the mix monomer charging of acid or ester.

Finish the preferred about 2.5 moles diol component of about 1.05-that uses: 1 moles of dicarboxylic acids component by ester exchange reaction mechanism in order to guarantee the reaction that drives diol component and dicarboxylic acid component.Yet, it will be understood by those skilled in the art that diol component and dicarboxylic acid component's ratio is normally determined by the DESIGN OF REACTOR of the process that wherein reacts.

Preparing in the sulfonic polyester by direct esterification, that is, from the dicarboxylic acid component of acid, sulfonic polyester is produced in the reaction of the mixture by dicarboxylic acids or dicarboxylic acids and the mixture of diol component or diol component.The reaction carry out under the following conditions: the about 7kPa of pressure (gauge pressure) (1psig)-Yue 1379kPa (gauge pressure) (200psig), preferably less than 689kPa (100psig), with the sulfonic polyester product of production low molecular weight linearity or branch, it has the average degree of polymerization of about 1.4-about 10.The temperature of using between the direct esterification stage of reaction is generally about 180 ℃-Yue 280 ℃.Another scope is about 220 ℃-Yue 270 ℃.This low-molecular weight polymer can come polymerization by polycondensation reaction then.

Multi-component fiber of the present invention, supatex fabric and fibre also may comprise other conventional additives and composition, and it does not influence their final use nocuously.For example can use additive such as filler, surface friction modifiers, light and thermally stable agent, extrusion aid, antistatic additive, colouring agent, dyestuff, pigment, fluorescent whitening agent, antimicrobial, anti-fake mark, hydrophobic and hydrophilic reinforcing agent, viscosity modifier, slipping agent, flexibilizer, adhesion promoter etc.

The multicomponent fibre of our invention, supatex fabric and fibre do not require to exist additive, pigment for example, and filler, oil, wax or aliphatic acid surface layer (finish) are to stop the adhesion or the fusion of fiber during processing.Term " adhesion or fusion " as used in this article, is interpreted as being meant that fiber or fibre stick together or be fused into one, makes that fiber can not be processed or be used for its predetermined purpose.Adhesion and merge can be during the processing of fiber or fibre or the memory period in a couple of days or several weeks take place, and under heat, moist condition, increase the weight of.

In one embodiment of the present invention, multicomponent fibre, supatex fabric and fibre can comprise this antiblocking additive less than 10wt%, based on the gross weight of multicomponent fibre or fibre.For example, multicomponent fibre and fibre can comprise pigment or the filler less than 10wt%.In other example, multicomponent fibre, supatex fabric and fibre can comprise less than 9wt%, less than 5wt%, less than 3wt%, less than pigment or the filler of 1wt% and 0wt%, based on the gross weight of multicomponent fibre.Colouring agent is sometimes referred to as toner, can be added so that give the tone (hue) and/or the brightness (brightness) of the desired neutrality of sulfonic polyester.When coloured multicomponent fibre is expectation time, pigment or colouring agent can be added between diol monomer and dicarboxylic acid monomer's the stage of reaction in the sulfonic polyester reactant mixture, perhaps they can with preformed sulfonic polyester melt blending.The preferable methods of adding colouring agent is to use the colouring agent of the organic colored compound (it has active group) with heat endurance, makes colouring agent by combined polymerization and be incorporated in the sulfonic polyester, thereby improves its tone.For example, colouring agent, as dyestuff, it has reactive hydroxyl and/or carboxyl, includes but not limited to, and the anthraquinone of blue and red replacement can be incorporated in the polymer chain by copolymerization.

In one embodiment of the present invention, comprised in the multicomponent fibre the glass transition temperature (Tg) of sulfonic polyester be at least 57 ℃.The glass transition temperature (Tg) that has been found that at least 57 ℃ is particularly useful in multicomponent fibre, with prevent in spinning and batch (take up) during the adhesion and the fusion of multicomponent fibre.Therefore, In one embodiment of the present invention, use a kind of multicomponent fibre with shaping section to make supatex fabric, it comprises:

(A) glass transition temperature (Tg) is at least 57 ℃ the dispersible sulfonic polyester of water, and this sulfonic polyester comprises:

(i) residue of one or more dicarboxylic acids;

The about 40mol% of (ii) about 4-, based on total repetition unit, the residue of at least a sulfomonomer, one or more sulfonate group that it has 2 functional groups and is attached to aromatics or cyclic aliphatic ring, wherein this functional group is a hydroxyl, carboxyl or its combination;

(iii) one or more glycol residues, wherein 25mol% at least based on the total diol residue, is poly-(ethylene glycol) with following structure

H-(OCH ₂-CH ₂) _n-OH

Wherein n is the integer of 2-about 500; With

The (iv) about 25mol% of 0-, based on total repetition unit, have 3 or the residue of the branched monomer of above functional group, wherein this functional group is a hydroxyl, carboxyl or its combination; With

(B) a plurality of sections (segment), it comprises the polymer that can not disperse with immiscible one or more water of sulfonic polyester, wherein this section (segment) is isolated from each other basically by the sulfonic polyester between described section (segment);

Wherein fiber has fabric of island-in-sea type or fan cake type (segmented pie) section.

Dicarboxylic acids, glycol, sulfonic polyester, sulfomonomer and branched monomer residue, foregoing, be used for other embodiment of the present invention.For multicomponent fibre, advantageously the Tg of sulfonic polyester is at least 57 ℃.Can be at least 60 ℃ by our sulfonic polyester of multicomponent fibre or the further example of the glass transition temperature that the sulfonic polyester blend demonstrates, at least 65 ℃, at least 70 ℃, at least 75 ℃, at least 80 ℃, at least 85 ℃ and at least 90 ℃.Further, for obtaining to have the sulfonic polyester of at least 57 ℃ Tg, can use the blend of one or more sulfonic polyesters to obtain to have the sulfonic polyester blend of desirable T g with the ratio that changes.The weighted average of glass transition temperature that can be by using the sulfonic polyester component calculates the Tg of sulfonic polyester blend.For example, Tg is that 48 ℃ sulfonic polyester can be that (wt: it was about 61 ℃ sulfonic polyester blend that ratio blend wt) obtains Tg with 25: 75 for another sulfonic polyester of 65 ℃ with Tg.

In another embodiment of the present invention, the dispersible sulfonic polyester component of the water of multicomponent fibre has presented various performances, and it allows at least a in following:

(A) multicomponent fibre be spun to expectation low dawn number and

(B) multicomponent fibre is that heat can formalize, thereby obtains a kind of stable, firm supatex fabric.Use has the sulfonic polyester of certain melt viscosity and sulfomonomer residue level, has obtained wondrous and beat all result in promoting these purposes.

Therefore, in this embodiment of the present invention, used a kind of multicomponent fibre, it has the shaping section, comprising:

(A) the dispersible sulfonic polyester of at least a water; With

(B) a plurality of territories (domains), described territory comprises the polymer that can not disperse with immiscible one or more water of sulfonic polyester, wherein said territory is isolated from each other basically by the described sulfonic polyester between described territory,

Wherein the first dawn number that spins of this multicomponent fibre is less than about 6 filament deniers;

Wherein the dispersible sulfonic polyester of water demonstrate less than about 12,000 the pool melt viscosity, measure under the strain rate of 1 radian per second at 240 ℃ and

Wherein sulfonic polyester comprises the residue less than at least a sulfomonomer of about 25mol%, based on the total mole number of diacid or glycol residue.

The melt viscosity of the sulfonic polyester that uses in these multicomponent fibres is usually less than about 12,000 pools.Other scope of the melt viscosity of sulfonic polyester is less than 10,000 pools, less than 6,000 with less than 4,000 pools, measures in 240 ℃ and 1 radian per second shear rate.In another aspect, sulfonic polyester demonstrates such melt viscosity: about 12000 pools of about 1000-, and about 6000 pools of about 2000-, about 4000 pools of about 2500-are measured in 240 ℃ and 1 radian per second shear rate.Before measuring viscosity, sample 60 ℃ in vacuum drying oven dry 2 days.Melt viscosity is to use flow graph to measure, and with the 1mm gap setting, it has the parallel discs geometry of 25mm diameter.Dynamically frequency sweep (dynamic frequency sweep) is to carry out under strain rate is the condition of 1-400 radian per second and 10% strain amplitude.Under the condition of the strain rate of 240 ℃ and 1 radian per second, measure viscosity then.

The level of sulfomonomer residue of sulfopolyester polymer that is used for this embodiment of the present invention perhaps, less than 20mol%, is reported with the percentage of total diacid in the sulfonic polyester or glycol residue normally less than about 25mol%.Other scope of the level of the sulfomonomer residue in the sulfopolyester polymer is the about 20mol% of about 4-, the about 12mol% of about 5-, the about 10mol% of about 7-.This embodiment on the other hand in, be used for one or more sulfonate group that sulfomonomer of the present invention can have 2 functional groups and be attached to aromatics or cyclic aliphatic ring, wherein this functional group is a hydroxyl, carboxyl or its combination, for example, sodium is for the sulfoisophthalic acid monomer.

Except that foregoing sulfomonomer, sulfonic polyester can comprise the residue of one or more dicarboxylic acids, one or more glycol residues, and wherein 25mol% at least based on the total diol residue, is poly-(ethylene glycol) with following structure

H-(OCH ₂-CH ₂) _n-OH

Wherein n is integer and the about 20mol% of 0-of 2-about 500, based on total repetition unit, have 3 or the residue of the branched monomer of above functional group, wherein this functional group is a hydroxyl, carboxyl or its combination.

In one embodiment of the present invention, sulfonic polyester comprises about 80-96mol% dicarboxylic acids residue, about 4-about 20mol% sulfomonomer residue and 100mol% glycol residue (total mol% is 200%, i.e. 100mol% diacid and 100mol% glycol).More particularly, the dicarboxylic acids of sulfonic polyester partly comprises about 60-80mol% terephthalic acid (TPA), and the 5-sodium of about 0-30mol% M-phthalic acid and about 4-20mol% is for sulfoisophthalic acid (5-SSIPA).Glycol moiety comprises about 0-50mol% diethylene glycol (DEG) and about 50-100mol% ethylene glycol.Hereinafter set forth exemplary preparation according to this embodiment of the present invention.

	About mol% (based on total mole of glycol or diacid residue)
		Terephthalic acid (TPA)	71
M-phthalic acid	20	Terephthalic acid (TPA)	71

5-SSIPA	9
5-SSIPA	9	Diethylene glycol (DEG)	35
Ethylene glycol	65	Diethylene glycol (DEG)	35

The component that the water of multicomponent fibre can not disperse can comprise any in the polymer that described those water can not disperse herein.The spinning of multicomponent fibre also can be carried out according to described any method herein.Yet the improved rheological equationm of state of multicomponent fibre according to this aspect of the invention provides the draw speed that improves.When the dispersible sulfonic polyester of water has less than about 12, the melt viscosity of 000 pool, measure under the strain rate of 1 radian per second at 240 ℃, and wherein sulfonic polyester comprises the residue less than at least a sulfomonomer of about 25mol%, total mole number based on diacid or glycol residue, and when being extruded with production multicomponent extrudate, use any method disclosed herein, with the speed at least about 2000m/min, the multicomponent extrudate can be melted stretching to produce this multicomponent fibre.This embodiment on the other hand in, the multicomponent extrudate can be melted stretching with the speed in the following scope: at least about 3000m/min, at least about 4000m/min, or at least about 4500m/min.Though be not intended to accept the constraint of opinion theory, cause at least some oriented crystalline degree in the component that the water at multicomponent fibre can not disperse at these speed fusion drawn multicomponent extrudates.This oriented crystalline degree can improve the DIMENSIONAL STABILITY of the supatex fabric of being made by multicomponent fibre during subsequent processing.

(have by such sulfonic polyester less than about 12, the melt viscosity of 000 pool, measure under the strain rate of 1 radian per second at 240 ℃, and wherein sulfonic polyester comprises the residue less than at least a sulfomonomer of about 25mol%, based on the total mole number of diacid or glycol residue) another advantage of the multicomponent extrudate produced is that it can be melted to be stretched to and just spins the multicomponent fibre of dawn number (as-spun denier) less than 6 filament deniers.Other scope of multicomponent fibre size comprises just spins the dawn number less than 4 filament deniers with less than 2.5 filament deniers.

Multicomponent fibre comprises a plurality of sections (segment) or the territory of the polymer that can not disperse with immiscible one or more water of sulfonic polyester, and wherein said section (segment) or territory are isolated from each other basically by the sulfonic polyester between described section (segment) or territory.As used in this article, term " substantial barrier ", intention is meant that section (segment) or territory are separated from each other, thereby when removing sulfonic polyester, allows section (segment), territory to form independent fiber.For example, section (segment) or territory can contact with each other, for example, and with fan cake type (segmented pie) configuration, but by impacting or when removing sulfonic polyester, can dividing and split.

In multicomponent fibre of the present invention, the weight ratio of the polymers compositions that sulfonic polyester and water can not disperse is generally about 60: about 2: 98 of 40-, perhaps, and in another example, about 50: about 5: 95 of 50-.Usually, sulfonic polyester accounts for the 50wt% of multicomponent fibre gross weight or following.

Section of multicomponent fibre (segment) or territory can comprise the polymer that one or more (one of more) water can not disperse.The example that can be used for the polymer that the water in the section (segment) of multicomponent fibre can not disperse is including, but not limited to polyene footpath, polyester, polyamide, polyactide, polycaprolactone, Merlon, polyurethane and polyvinyl chloride.For example, the polymer that water can not disperse can be polyester such as polyethylene terephthalate, polybutylene terephthalate, poly-cyclohexane cyclohexanedimethanodibasic hexamethylene diester, poly terephthalic acid hexamethylene diester, polytrimethylene terephthalate etc.

In one embodiment of the present invention, the polymer that water can not disperse is a polyethylene terephthalate, its logarithmic viscosity number is less than 0.6dL/g, at the measurement of concetration of 25 ℃ of polyethylene terephthalate of about 0.5g in the solution of the phenol/tetrachloroethane solvent of 60/40 weight portion and in the solvent of 100mL.Other scope is less than 0.55dL/g, less than 0.4dL/g with less than 0.3dL/g.PET with this logarithmic viscosity number can produce the improved supatex fabric that has fiber with excellent entanglement and less bulk fibre (loose fibers) on the surface of supatex fabric.

In another example, the polymer that water can not disperse can be biological decomposable (biodistintegratable), and as that measure and/or biodegradable according to Deutsche industry norm (DIN) 54900, as according to the ASTM standard method, D6340-98 measures.The example of biodegradable polyester and polyester blend is disclosed in United States Patent (USP) 5,599,858; 5,580,911; 5,446,079; With 5,559, in 171.Term " biodegradable (biodegradable) ", as used in this article, be related to the polymer that water of the present invention can not disperse, be interpreted as being meant polymer suitable and significantly in the time span in for example degraded (degrade) in compost (composting) environment under the ambient influnence, for example, by the ASTM standard method that is entitled as " Standard Test Methods for Determining AerobicBiodegradation of Radiolabeled Plastic Materials in an Aqueous or CompostEnvironment (being used to measure the standard method of test of the aeration and biological degraded of radiolabeled plastic material in moisture or compost environment) ", D6340-98 is defined.The polymer that water of the present invention can not disperse also can be " biological decomposable (biodisintegratable) ", and this is meant polymer incoherent in compost environment easily (fragment), and is for example defined by Deutsche industry norm (DIN) 54900.For example, biodegradable polymer under the effect of heat, water, air, microorganism and other factors, reduces aspect molecular weight in environment at first.This reduction of molecular weight causes the loss of physical property (toughness) and usually causes fibrous fracture.In case the molecular weight of polymer is enough low, so monomer and oligomer are assimilated by Institute of Micro-biology.In aerobic environment, these monomers or oligomer finally are oxidized to CO ₂, H ₂O and new cellular biomass.In anaerobic environment, monomer or oligomer finally are converted into CO ₂, H ₂, acetate (ester), methane and cellular biomass.

For example, the polymer that water can not disperse can be an aliphatic-aromatic polyesters, and it is abbreviated as " AAPE " in this article.Term " aliphatic-aromatic polyesters " as used in this article, is meant the polyester that comprises from the mixture of the residue of aliphatic series or cycloaliphatic dicarboxylic acid or two pure and mild aromatic dicarboxylic acids or glycol.Term " non-aromatics " as used in this article, for dicarboxylic acids of the present invention and diol monomer, is meant that the carboxyl of monomer or hydroxyl do not connect by aromatic ring.Therefore for example, adipic acid does not comprise aromatic ring in its main chain (carbon atom chain that promptly connects hydroxy-acid group), is " non-aromatics ".By contrast, term " aromatics " is meant that in main chain dicarboxylic acids or glycol comprise aromatic ring, for example, and terephthalic acid (TPA) or 2,6-naphthalenedicarboxylic acid." non-aromatics ", therefore, intention comprises aliphatic series and cyclo-aliphatic structure, for example, two pure and mild dicarboxylic acids, it comprises the straight or branched of forming carbon atom or circulus as main chain, and described composition carbon atom can be saturated or alkane in nature, and is undersaturated, promptly comprise non-aromatics carbon-to-carbon double bond, perhaps acetylene series promptly, comprises carbon-to-carbon triple bond.Therefore, in the scope of specification of the present invention and claim, non-aromatics intention comprises the chain structure (being referred to herein as " aliphatic series ") of linear and branch and circulus (be referred to herein as " alicyclic () " or " cyclic aliphatic () ").Term " non-aromatics ", yet, being not intended to get rid of any aromatic substituent, it can be connected to the main chain of aliphatic series or cycloaliphatic diol or dicarboxylic acids.In the present invention, the bifunctional carboxylic acid usually is an aliphatic dicarboxylic acid, for example adipic acid, or aromatic dicarboxylic acid, for example terephthalic acid (TPA).The difunctionality hydroxy compounds can be a cycloaliphatic diol, 1,4 cyclohexane dimethanol for example, the aliphatic diol of linearity or branch, for example 1,4-butanediol, perhaps aromatic diol, for example quinhydrones.

AAPE can be the random copolyesters of linearity or branch and/or the copolyesters of chain extension, it comprises the glycol residue, that described glycol residue comprises is one or more replacements or unsubstituted, the residue of the glycol of linearity or branch, and described glycol is selected from the aliphatic diol that comprises about 8 carbon atoms of 2-, the polyalkylene ether two pure and mild cycloaliphatic diols that comprise about 12 carbon atoms of about 4-that comprise 2-8 carbon atom.The glycol that replaces usually, will comprise about 4 substituting groups of 1-, and it is independently selected from halogen, C ₆-C ₁₀Aryl and C ₁-C ₄Alkoxyl.The example of operable glycol is including, but not limited to ethylene glycol, diethylene glycol (DEG), propylene glycol, 1, ammediol, 2,2-dimethyl-1, ammediol, 1,3 butylene glycol, 1, the 4-butanediol, 1,5-pentanediol, 1,6-hexylene glycol, polyethylene glycol, diethylene glycol (DEG), 2,2,4-trimethyl-1,6-hexylene glycol, thiodiethanol, 1,3-cyclohexanedimethanol, 1, the 4-cyclohexanedimethanol, 2,2,4,4-tetramethyl-1,3-cyclobutanediol, triethylene glycol and tetraethylene glycol, preferred glycol comprises that one or more are selected from 1, the 4-butanediol; 1, ammediol; Ethylene glycol; 1, the 6-hexylene glycol; Diethylene glycol (DEG); Or the glycol of 1,4 cyclohexane dimethanol.AAPE also comprises the diacid residue, it comprises the about 99mol% of about 3 5-, total mole number based on the diacid residue, the residue of non-aromatic dicarboxylic acid one or more replacements or unsubstituted, linearity or branch, described dicarboxylic acids is selected from aliphatic dicarboxylic acid that comprises about 12 carbon atoms of 2-and the cycloaliphatic acids that comprises about 10 carbon atoms of about 5-.The non-aromatic dicarboxylic acid that replaces usually, will comprise about 4 substituting groups of 1-, and it is selected from halogen, C ₆-C ₁₀Aryl and C ₁-C ₄Alkoxyl.The limiting examples of non-aromatic diacid comprises malonic acid, butanedioic acid, glutaric acid, adipic acid, pimelic acid, azelaic acid, decanedioic acid, fumaric acid, 2,2-dimethylated pentanedioic acid, suberic acid, 1,3-pentamethylene dicarboxylic acids, 1,4-cyclohexane dicarboxylic acid, 1,3-cyclohexane dicarboxylic acid, diglycolic acid, itaconic acid, maleic acid and 2,5-norcamphane dicarboxylic acids.Unless outside the aromatic dicarboxylic acid, AAPE comprises the about 65mol% of about 1-, based on the total mole number of diacid residue, one or more replacements or the unsubstituted residue that comprises the aromatic dicarboxylic acid of about 10 carbon atoms of 6-.Use under the situation of the aromatic dicarboxylic acid that replaces therein, they will usually comprise about 4 substituting groups of 1-, and it is selected from halogen, C ₆-C ₁₀Aryl and C ₁-C ₄Alkoxyl.The limiting examples that can be used for the aromatic dicarboxylic acid among our AAPE of invention is the salt and 2 of terephthalic acid (TPA), M-phthalic acid, 5-sulfoisophthalic acid, the 6-naphthalene dicarboxylic acids.More preferably, non-aromatic dicarboxylic acid will comprise adipic acid, and aromatic dicarboxylic acid will comprise terephthalic acid (TPA), and glycol will comprise 1, the 4-butanediol.

Other is by those of following two pure and mild dicarboxylic acids (or its become the equivalent of polyester, as diester) preparation for the feasible composition of the AAPE of our invention, by following mole percent, based on the diacid component of 100mol% and the diol component of 100mol%:

(1) glutaric acid (about 30-about 75%); Terephthalic acid (TPA) (about 25-about 70%); 1,4-butanediol (about 90-100%); With modification glycol (0-about 10%);

(2) butanedioic acid (about 30-about 95%); Terephthalic acid (TPA) (about 5-about 70%); 1,4-butanediol (about 90-100%); With modification glycol (0-about 10%); With

(3) adipic acid (about 30-about 75%); Terephthalic acid (TPA) (about 25-about 70%); 1,4-butanediol (about 90-100%); With modification glycol (0-about 10%).

The modification glycol preferably is selected from 1,4 cyclohexane dimethanol, triethylene glycol, polyethylene glycol and neopentyl glycol.Most preferred AAPE is the copolyesters of linear, branch or chain extension, and it comprises the about 60mol% adipic acid of about 50-residue, about 40-about 50mol% terephthalic acid (TPA) residue and at least 95mol% 1,4-butanediol residue.More preferably, the adipic acid residue accounts for the about 60mol% of about 55-, and the terephthalic acid (TPA) residue accounts for the about 45mol% of about 40-and the glycol residue comprises 1 of about 95mol%, 4-butanediol residue.This composition is commercially available getting, with trade mark EASTAR

Copolyesters is available from Eastman Chemical Company, Kingsport, TN and with trade mark

Available from BASF Corporation.

In addition, the specific example of preferred AAPE comprises poly-(tetramethylene glutarate-co-terephthalate), it comprises (a) 50mol% glutaric acid residue, 50mol% terephthalic acid (TPA) residue, and 100mol%1,4-butanediol residue, (b) 60mol% glutaric acid residue, 40mol% terephthalic acid (TPA) residue, and 100mol%1,4-butanediol residue or (c) 40mol% glutaric acid residue, 60mol% terephthalic acid (TPA) residue, and 100mol%1,4-butanediol residue; Poly-(tetramethylene succinate-co-terephthalate), it comprises (a) 85mol% butanedioic acid residue, 15mol% terephthalic acid (TPA) residue, and 100mol%1,4-butanediol residue or (b) 70mol% butanedioic acid residue, 30mol% terephthalic acid (TPA) residue, and 100mol%1,4-butanediol residue; Poly-(ethylidene succinic acid ester-co-terephthalate), it comprises 70mol% butanedioic acid residue, 30mol% terephthalic acid (TPA) residue and 100mol% ethylene glycol residue; With poly-(tetramethylene adipate ester-co-terephthalate), it comprises (a) 85mol% adipic acid residue, 15mol% terephthalic acid (TPA) residue, and 100mol%1,4-butanediol residue; Or (b) 55mol% adipic acid residue, 45mol% terephthalic acid (TPA) residue, and 100mol%1,4-butanediol residue.

AAPE preferably includes about 1,000 repetitive of about 10-, preferably, and about 600 repetitives of about 15-.The AAPE logarithmic viscosity number can be the about 2.0dL/g of about 0.4-, the about 1.6dL/g of perhaps more preferably about 0.7-, measure as the copolyesters that uses following concentration 25 ℃ temperature: the solution of phenol/tetrachloroethanes (60/40, calculate by weight) of 0.5 gram copolyesters/100ml.

AAPE randomly, can comprise the residue of branching agent.The mole percent scope of branching agent is the about 2mol% of about 0-, and about 1mol% of preferably about 0.1-and the about 0.5mol% of 0.1-most preferably from about are based on the total mole number (depending on whether branching agent comprises carboxyl or hydroxyl) of diacid or glycol residue.Branching agent preferably has following weight average molecular weight: about 50-is about 5000, and more preferably about 92-about 3000 and degree of functionality are about 3-about 6.The polybasic carboxylic acid that branching agent for example, can be a polyalcohol with 3-6 hydroxyl, have 3 or 4 carboxyls (or becoming ester equivalent group) or have altogether the esterification residue of the carboxylic acid of 3-6 hydroxyl and carboxyl.In addition, during extruding, reaction can make the AAPE branch by adding peroxide.

Each section (segment) of the polymer that water can not disperse can be aspect fineness with the different of other and can be aligned to any shaping well known by persons skilled in the art or the geometric shape of processing section.For example, the polymer that sulfonic polyester and water can not disperse can be used to prepare the multicomponent fibre with following processing geometry, for example, parallel type, " fabric of island-in-sea type ", fan cake type (segmented pie), but other Schizoid (splitables), skin/core pattern, other configuration perhaps well known by persons skilled in the art.Other multicomponent configuration also is possible.Remove a side of parallel type subsequently, " sea " of fabric of island-in-sea type or the part of " cake " can obtain very thin fiber.The method for preparing multicomponent fibre also is that those skilled in the art are well-known.In multicomponent fibre, the content of sulfonic polyester fiber of the present invention can be about 90wt% of about 10-and the skin portion that will be generally used for skin/core fibre.Other component can be from various other polymeric materials, for example, and polyethylene terephthalate, polybutylene terephthalate, polytrimethylene terephthalate, polyactide or the like and polyene footpath, cellulose esters, and polyamide.Usually, when using water-fast or during polymer that water can not disperse, the bi-component of gained or multicomponent fibre are not that complete water is dispersible.The parallel type combination that has significant difference aspect thermal contraction can be used for forming helix-coil.If curl is expectation, and sawtooth or stuffer box crimping are applicable to many application usually.If second polymers compositions is arranged in the core of skin/core configuration, this core randomly can be stabilized.

Sulfonic polyester is particularly useful for having the fiber of " fabric of island-in-sea type " or " fan cake type (segmented pie) " section, because they only require neutrality or omit acidity (promptly, " soft " water) disperse, compare the solution that contains caustic alkali (caustic), the latter is required sometimes to remove other water dispersible polymers from multicomponent fibre.Therefore, our invention be multicomponent fibre on the other hand, it comprises:

(i) one or more residues of the M-phthalic acid of the about 96mol% of about 50-or terephthalic acid (TPA) are based on the total acid residue;

The about 30mol% of (ii) about 4-, based on the total acid residue, sodium for the residue of sulfoisophthalic acid;

H-(OCH ₂-CH ₂) _n-OH

Wherein n is the integer of 2-about 500;

The (iv) about 20mol% of 0-, based on total repetition unit, have 3 or the residue of the branched monomer of above functional group, wherein this functional group is a hydroxyl, carboxyl or its combination; With

Wherein fiber has fabric of island-in-sea type or fan cake type (segmented pie).

The polymer that dicarboxylic acids, glycol, sulfonic polyester, sulfomonomer, branched monomer residue and water can not disperse is foregoing.For multicomponent fibre, advantageously the Tg of sulfonic polyester is at least 57 ℃.Sulfonic polyester can be the blend of single sulfonic polyester or one or more sulfopolyester polymers.The further example of the glass transition temperature that can be demonstrated by sulfonic polyester or sulfonic polyester blend is at least 65 ℃, at least 70 ℃, and at least 75 ℃, at least 85 ℃ and at least 90 ℃.For example, sulfonic polyester can comprise the residue of the diethylene glycol (DEG) of one or more residues of the M-phthalic acid of the about 96mol% of about 75-or terephthalic acid (TPA) and the about 95mol% of about 25-.As indicated above, the example of the polymer that water can not disperse is polyene footpath, polyester, polyamide, polyactide, polycaprolactone, Merlon, polyurethane and polyvinyl chloride.In addition, the water polymer that can not disperse can be biodegradable or biological decomposable (biodisintegratable).For example, the polymer that water can not disperse can be aliphatic-aromatic polyesters, and is foregoing.

Multicomponent fibre can be prepared by many methods well known by persons skilled in the art.In one embodiment of the present invention, produced multicomponent fibre by the following method with shaping section, this method comprises: with glass transition temperature (Tg) at least 57 ℃ the dispersible sulfonic polyester of water with become fiber with polymer spinning that immiscible one or more water of sulfonic polyester can not disperse, described sulfonic polyester comprises:

(i) residue of one or more dicarboxylic acids;

H-(OCH ₂-CH ₂) _n-OH

Wherein n is the integer of 2-about 500; With

The (iv) about 25mol% of 0-, based on total repetition unit, have 3 or the residue of the branched monomer of above functional group, wherein this functional group is a hydroxyl, carboxyl or its combination;

Wherein this fiber has a plurality of section (segment) of the polymer that water can not disperse and this sections (segment) of comprising and is isolated from each other basically by the sulfonic polyester between described section (segment).

For example, multicomponent fibre can prepare like this, be included in the polymer that fusion sulfonic polyester and one or more water can not disperse in the independent extruder, and independent polymer flow is imported a spinnerets or the extrusion die with a plurality of distribution flow paths, the polymers compositions that makes water to disperse forms little section (segment) or thin strand, and the latter is isolated from each other basically by intervenient sulfonic polyester.The section of this fiber can be for example, to fan cake type (segmentedpie) structure or island type structure.In another example, the polymer that sulfonic polyester and one or more water can not disperse is supplied to the spinnerets aperture individually, extrudes with the core-skin type form subsequently, wherein, the polymer that water can not disperse forms " core ", and the latter is centered on by sulfonic polyester " skin " polymer basically.Under the situation of this concentric fibers, the aperture of supplying with " core " polymer is positioned at the center of spinning aperture outlet, and the flox condition of core polymer fluid keeps the concentricity of two components when strictly being controlled with convenient spinning.The change in spinnerets aperture makes it possible to obtain the different cores and/or the shape of skin in the fiber section.In another example, multicomponent fibre with parallel type section or configuration can be produced like this, comprise the polymer that can not disperse by dispersible sulfonic polyester of aperture co-extrusion water outlet and water respectively, and compile each independently polymer stream and below spinning plate surface, be merged into parallel type with form in conjunction with logistics with substantially the same speed; Or (2) by the aperture compiled in the spinnerets surface with substantially the same speed two kinds of polymer streams of charging respectively, thereby be merged into parallel type with form in the spinnerets surface in conjunction with logistics.In two kinds of situations, merging the some place, the speed of each polymer stream is determined by its measuring pump speed, aperture number and port size.

The polymer that dicarboxylic acids, glycol, sulfonic polyester, sulfomonomer, branched monomer residue and water can not disperse is foregoing.The glass transition temperature of sulfonic polyester is at least 57 ℃.The further example of the glass transition temperature that can be demonstrated by sulfonic polyester or sulfonic polyester blend is at least 65 ℃, at least 70 ℃, and at least 75 ℃, at least 85 ℃ and at least 90 ℃.In an example, sulfonic polyester can comprise the M-phthalic acid of the about 96mol% of about 50-or one or more residues of terephthalic acid (TPA), based on the total acid residue; With the about 30mol% of about 4-, based on the total acid residue, sodium for the residue of sulfoisophthalic acid; With the about 20mol% of 0-, based on total repetition unit, have 3 or the residue of the branched monomer of above functional group, wherein this functional group is a hydroxyl, carboxyl or its combination.In another example, sulfonic polyester can comprise the residue of the diethylene glycol (DEG) of one or more residues of the M-phthalic acid of the about 96mol% of about 75-or terephthalic acid (TPA) and the about 95mol% of about 25-.As indicated above, the example of the polymer that water can not disperse is polyene footpath, polyester, polyamide, polyactide, polycaprolactone, Merlon, polyurethane and polyvinyl chloride.In addition, the water polymer that can not disperse can be biodegradable or biological decomposable (biodisintegratable).For example, the polymer that water can not disperse can be aliphatic-aromatic polyesters, and is foregoing.The example of shaping section is including, but not limited to fabric of island-in-sea type, parallel type, and core-skin type is perhaps fanned cake type (segmented pie) configuration.

In another embodiment of the present invention, produced multicomponent fibre by the following method with shaping section, this method comprises: the dispersible sulfonic polyester of at least a water of spinning and the polymer that can not disperse with immiscible one or more water of sulfonic polyester are to produce multicomponent fibre, wherein multicomponent fibre has a plurality of territories, described territory comprises the polymer that water can not disperse, and described territory is isolated from each other basically by the described sulfonic polyester between described territory; Wherein the dispersible sulfonic polyester of water demonstrates less than about 12, the melt viscosity of 000 pool, measure under the strain rate of 1 radian per second at 240 ℃, wherein sulfonic polyester comprises the residue less than at least a sulfomonomer of about 25mol%, based on the total mole number of diacid or glycol residue; Wherein the first dawn number that spins of multicomponent fibre is less than about 6 filament deniers.

At preamble the sulfonic polyester that is used for the polymer that these multicomponent fibres and water can not disperse has been discussed in the present invention.

In another embodiment of the present invention, can produce multicomponent fibre by the following method with shaping section, this method comprises:

(A) extrude the dispersible sulfonic polyester of at least a water and the polymer that can not disperse with immiscible one or more water of described sulfonic polyester to produce the multicomponent extrudate, wherein the multicomponent extrudate has a plurality of territories, described territory comprises the polymer that water can not disperse, and described territory is isolated from each other basically by the described sulfonic polyester between described territory; With

(B) with at least about the speed fusion drawn multicomponent extrudate of 2000m/min to produce this multicomponent fibre.

The feature of this embodiment is that also described method comprises with the step at least about the speed fusion drawn multicomponent extrudate of 2000m/min, more preferably, and at least about 3000m/min and 4500m/min at least most preferably.

Usually, when leaving spinnerets, by the air cross-flow, fiber is by quenching, so fiber solidifies.In this step, various arrangements (finish) and starching (size) can be applied to fiber.Cooled fibers usually, is stretched subsequently and rolls on winding off spindle.Other additive can add in the surface layer (finish) with effective dose, for example emulsifying agent, antistatic agent, antimicrobial, defoamer, lubricant, heat stabilizer, UV stabilizer etc.

Randomly, drawing of fiber can veining and is twined to form fluffy continuous filament yarn.A this step technology is well known in the art, and is called spinning-stretching-veining.Other embodiment comprises flat filaments (non-veining) yarn, and perhaps staple is curling or curl.

The step of the inventive method (A) comprises collects multicomponent fibre to form nonwoven web.Multicomponent fibre by preceding method production can be collected in the mode of producing nonwoven web, makes that the carrier of multicomponent fibre is optional.This can finish by any methods known in the art.For example, multicomponent fibre can stand such method such as machinery sewing (mechanicalneedling), chemical bonding (chemical bindng), hot calendering (thermally calendaring), ultrasonic fusion (ultrasonic fusing) or water entanglement (hydroentangling), so that enough invigoration effects (consolidation) are provided, wherein the carrier of multicomponent fibre is optional.The example of machinery sewing is needle point method (needle punching).

In one embodiment of the present invention, when selecting water to tangle to strengthen or during, in this step, only carry out enough water and tangle and make that carrier is not that multicomponent fibre is needed in conjunction with multicomponent fibre.In one embodiment of the present invention, the quantity of the water entanglement energy that is spent in this method can be about 20%-about 50% of the water entanglement energy that spent in the step (C) of this method.As discussing hereinafter, in the present invention, the water after sulfonic polyester is removed tangles, and (the step C) of described method is that wherein most of energy is spent so that make the multicomponent fibre interlocking to produce the step of supatex fabric.Because fiber is trickleer, when sulfonic polyester was removed, this provided improved supatex fabric and has needed less water entanglement energy, than the legacy system of water entangled fiber before sulfonic polyester is removed.

In another embodiment of the present invention, extruding technology can be utilized so that from being used to make the nonwoven web that the employed material of multicomponent fibre itself comes production stage (A), eliminated the multicomponent fibre production stage thus.These methods comprise spunbond and meltblowing method.The polymer that spunbond method can not be disperseed the dispersible sulfonic polyester of water and water in the following manner directly shifts (tranforms) in nonwoven web: extrude multicomponent fibre, with its orientation bunchy or bunch, its shop layer is being carried on the screen cloth, and need not independent fiber production step.In conventional method, multicomponent fibre is configured as fabric by independent method then at first by spinning and collection.Therefore, dispersible sulfonic polyester of water and the water polymer that can not disperse obtains the nonwoven web of step (A) through spunbond method.Fig. 1 has shown spunbond method.In meltblowing method, the polymer that dispersible sulfonic polyester of water and water can not disperse be heated to liquid state and when its when the extrusion cavities, its in about 250 to 500 ℃ of injections with velocity of sound air.The air logistics of fast moving stretches molten polymer and it is solidified to produce thin multicomponent fibre.Multicomponent fibre separates with the air logistics with the form of entangled web then and push nonwoven web with production stage (A) between warm-up mill.

Usually, the weight of nonwoven web can be about 10 gram/m ²-Yue 800 gram/m ²Other scope is 10 gram/m ²-600 gram/m ², 10 gram/m ²-400 gram/m ², 50 gram/m ²-300 gram/m ²Gram/m ²And about 50 gram/m ²-Yue 150 gram/m ²

The step of the inventive method (B) is included in and under enough extraction temperature and the pressure nonwoven web is contacted with water and remove the dispersible sulfonic polyester of water of a part, forms microfiber webs thus.Typically, multicomponent fibre can contact with water under about 20 ℃-Yue 100 ℃ extraction temperature.Other extracts temperature range is 25 ℃-Yue 100 ℃ and about 40 ℃-Yue 90 ℃.

Extracting temperature can limit by following program.The nonwoven web of being made up of the multicomponent fibre with the dispersible sulfonic polyester content of known water is weighed and is become to bring to metal caul subsequently and cover with 100-200 purpose stainless steel cloth at the top.The backboard that will have supatex fabric under about 20 ℃-Yue 60 ℃ probe temperature places the deionization water-bath to reach 10 minutes and extracts the dispersible sulfonic polyester of water.After conditioning, from water, take out sample, by the absorbability towel being placed more than the mesh and pushing and remove excessive water.Fabric webs after the conditioning is being forced in the air-oven dry and measure last weight at 60 ℃.Because extracting the loss in weight that causes calculates with the form of the percentage of starting weight.The temperature of opsonic water is removed during this temperature is being nursed one's health greater than 80% sulfopolyester polymer in original fibers, is designated as sulfonic polyester and extracts temperature.

Usually, the temperature of water, pressure, contact time are such, make to have removed the dispersible sulfonic polyester of water, and nonwoven web have kept the sufficiently complete as structure.The pressure of water can be the about 600barr of about 30barr-.Other pressure limit is 50barr-300barr.

In one embodiment of the present invention, nonwoven web can contact the time that is enough to remove the dispersible sulfonic polyester of whole water contained in the multicomponent fibre of the about 100wt% of about 30wt%-that reaches with water.In another embodiment of the present invention, from nonwoven web, remove greater than the dispersible sulfonic polyester of whole water of 90wt%.In another embodiment, remove from nonwoven web greater than the dispersible sulfonic polyester of whole water of 95wt%.

In another embodiment, nonwoven web contacts the about 600 seconds time of about 10-that reaches with water, and wherein the dispersible sulfonic polyester of water is dispersed or dissolves.

After removing sulfonic polyester, the polymer microfibers that remaining water can not disperse can have the average fineness less than the dawn number of 30% initial multicomponent fibre.The polymer microfibers that remaining water can not disperse usually will have such average fineness: 1d/f or following, usually, and 0.5d/f or following, perhaps more generally, 0.1d/f or following.

Usually, by any methods known in the art, nonwoven web contacts with water.For example, can use water ejector.In one embodiment of the present invention, can use 1-8 sprinkler head.The employed water yield be with the weight of nonwoven web before water contacts less than 500 times to less than 1000 times.

The washings of moisture dispersible sulfonic polyester can be recycled.In one embodiment of the present invention, 80% or more washings be recycled.This is suitable progress, because in the conventional method that is used for producing supatex fabric, washings can not be recycled usually, because the dispersible sulfonic polyester of water may occluding device and may be caused excessive wear and tear in machines.In another embodiment of the present invention, whole basically sulfonic polyesters are removed from washings.The sulfonic polyester method for recycling is described in the following document: U.S. patent application serial number 11/343,955, on January 31st, 2006 submitted to, Gupta, exercise question is " sulfonic polyester recirculation (SulfopolyesterRecovery) ", is incorporated herein by reference under its degree of not runing counter to statement herein.

Step (C) comprises that water entanglement microfiber webs is to produce supatex fabric.Usually, the water temperature during water tangles is less than 40 ℃.Pressure can be about 150 Ba-Yue 220 crust.In this water entanglement step, from microfiber webs, remove less than the dispersible sulfonic polyester of the water of 1wt%.In other embodiments of the present invention, the amount of the dispersible sulfonic polyester of water that is removed can be less than 0.8wt%, less than 0.5wt%, less than 0.25wt%, less than 0.1wt%, less than 0.08wt%, less than 0.05wt% with less than 0.02wt%, based on the weight of microfiber webs.Water from water entanglement step also can be recycled, as mentioned above.Because the dispersible sulfonic polyester of low-level water, sulfonic polyester may not be removed from washings before reusing.

In one embodiment of the present invention, carrying out water by water ejector tangles.The number of sprinkler head can be about 20 for 1-, or 2-about 15 or about 10 (individual) of 2-.Because significantly the sulfonic polyester of quantity is removed, fiber contained in the microfiber webs is trickle a lot, and during water entanglement step, has produced good supatex fabric, and it has fine and close configuration, and less fiber grinds loose (fraying) and bulk fibre.

In addition, water entanglement method of the present invention can be simplified, and than the non-woven water entanglement method of routine, wherein carried out water and tangle before removing the dispersible polymers that anhydrates.Because the polymer fiber that the water in microfiber webs can not disperse is trickleer, need less hydraulic pressure energy (hydraulic energy) to come entangled fiber.In addition, in the nonwoven processes of routine, water tangles and typically carried out before removing the dispersible sulfonic polyester that anhydrates, and frequently, need tangle by the further water after removing sulfonic polyester.Yet, in the present invention, under the situation that does not have further water entanglement step, can obtain high-quality supatex fabric.

In another embodiment of the present invention, a kind of method that is used to make supatex fabric is provided, it comprises:

(A) collect multicomponent fibre to form nonwoven web; Wherein multicomponent fibre comprises the polymer that dispersible sulfonic polyester of at least a water and at least a water can not disperse; Wherein multicomponent fibre has a plurality of territories, and described territory comprises the polymer that water can not disperse; Wherein said territory is isolated from each other basically by the dispersible sulfonic polyester of the water between described territory; With

(B) nonwoven web is contacted with water and remove the described sulfonic polyester of a part, form microfiber thus, and the microfiber of water entanglement simultaneously is to produce supatex fabric.

The aforementioned in this disclosure step (A) and (B) crossed.

Supatex fabric can experience heat setting step (heat setting), and described heat setting step comprises supatex fabric is heated to temperature at least about 100 ℃, more preferably at least about 120 ℃.The heat setting step has been alleviated internal fiber stress and has been helped to produce the fabric product of dimensionally stable.Preferably when the heat setting material is heated to its temperature that is heated to once more during described heat setting step, its surface area that demonstrates less than its initial surface area of about 5% shrinks.More preferably, shrink initial surface area, most preferably shrink less than about 1% less than about 2%.

Supatex fabric can randomly combine in the following manner: 1) poly-and interlocking in the mechanical fiber in fiber web or vexed smooth fabric; 2) the various technology of fiber fusion comprise the use binder fiber, utilize the thermoplastic properties of some polymer and blend polymer; 3) use binder resin such as starch, casein, cellulose derivative, or synthetic resin, as acrylic latex or urethane; 4) powder-stuck bond; Or 5) its combination.Fiber in the supatex fabric deposits with random fashion usually, but orientation in a direction is possible, uses one of said method to carry out combination/bonding subsequently.

The present invention has produced supatex fabric, and it can be used for clothes, curtain, upholstery and uniform.Supatex fabric can also be used for the personal care product, as but be not limited to rag, feminine hygiene, baby diaper, training pants, adult-incontinence underpants and hospital/surgery and other medical disposable product, as but be not limited to surgery apparel, gauze, bandage etc.Other is used including, but not limited to multi-layer nonwoven cloth, laminated thing and compound, protection fabric and layer, geotextile, industrial wipes and filter medium.Further, fibre can comprise the replacement insert that is used for various personal hygienes and cleaning products.Fibre of the present invention can with other may be water dispersible or may not be the dispersible material of water bonding, laminated, adhere to or use jointly.Fibre, for example, non-woven fabric layer can be bonded to material such as poly backing that flexible plastic film or water can not disperse.This assembly (assembly) for example, can be used as an assembly of disposable diaper.

Embodiment

Multicomponent fibre described in production following examples in the manner as described below and supatex fabric.The pilot-scale bicomponent spunbond production line that can produce 0.5 meter wide supatex fabric is used for the supatex fabric that spinning multicomponent fibre and production are used for listed embodiment.The simplification artwork of spunbond production line is shown among Fig. 1.The details of this method is described subsequently.

Use independent extruder and Spinning pumps to come the dispersible sulfonic polyester of fusion water and PET and it is metered in the bi-component spinning pack.An extruder fusion and be metered into the dispersible sulfonic polyester of water, and second extruder fusion and be metered into pet polymer.In this method,, and extrude the PET component 285 ℃ of melt temperatures at 260 ℃ the dispersible sulfonic polyester of melt temperature expressed water.Total polymer flow rate that merges be about 1.33kg/ minute, this feasible from the spinnerets with 2222 holes produce about 0.60 gram/hole/minute the average polymer flow velocity that leaves each nib.

Two polymer melt logistics enter fan cake type (segmented pie) the bi-component spinning pack of distribution polymer melt (by Hills Inc., Melbourne, FL. make), make that the form of molten material flows of final merging is 2222 multicomponent fibres with fan cake type (segmented pie) distribution of polymer.Salient angle (lobes) comprises the PET component, and the zone between these salient angles is by constituting with the dispersible sulfonic polyester of the water of PET coextrusion during this fibre spinning method.Spinnerets in this spinning pack is constructed by 2222 nibs, and described nib has 0.35 millimeter diameter separately.

Use compressed-air actuated getter assembly to be utilized so that form the logistics that flows downward at a high speed, its polymer melt logistics that is extruded that will leave spinnerets is drawn into thin multicomponent fibre.In embodiments of the present invention, apply enough air pressures and stretch multicomponent fibre to the fineness or the about 12 microns nominal filament diameter of about 8-of about 1.5 filament deniers of about 1.0-(dpf).

Drawing of fiber is listed on the collecting belt and forms continuous nonwoven web, wherein controls the density (basic weight) of nonwoven web by belt speed and rate of extrusion.Produce in an embodiment have about 150 grams of about 100-/square metre or the nonwoven web of typical as described basic weight.

Use hold-down roller (compacting roll) and batch platform (wind up station) has the slight compression nonwoven web of the multicomponent fibre of fanning cake type (segmented pie) fiber section structure with production scroll.Use calender to carry out compressing of nonwoven web to strengthen nonwoven web by enough point pressures that rolls in room temperature, make its can be on roller processed and unwinding so that further handle.

Nonwoven web by preceding method production uses the pilot-scale water entanglement production line (Fleissner of manufacturer, Engelsbach, Germany) with 5 water entanglement heads to come water to tangle subsequently.In an embodiment, use water entanglement head and pressure, utilize water entanglement equipment as different numbers illustrated among the embodiment.Water entanglement equipment has 3 water under high pressure entanglement heads, and it contacts nonwoven web, when it passes through under the water ejector that is supported by 103 mesh sieve guipures.First stature uses about only 30 crust hydraulic pressure as pre-wetting operation, and water 2 and 3 typical water of clinging at about 100-about 200 of tangling are depressed operation.The tangle water ejector of head of two final water can use vacuum in the drum that the water of the porous surface of water in water entanglement injector sucks drum is tangled to rouse when carrying, clash into nonwoven web when it has.These two final water entanglement injectors are operated under about 200 crust hydraulic pressure, and the injector contact is with respect to the fabric side of first three water entanglement injector institute contact side.

In each water tangles head, insert the injector band, its production line by the hole of retrofit constitutes, and the diameter in the hole of described retrofit is about 120 microns, is spaced apart about 0.8mm between the hole.The hydraulic pressure of about 200 crust on one side of the injector band in water tangles head makes the high velocity jet of water form in the hole separately.These high velocity water jets make the multicomponent fibre in the nonwoven web tangle, when described net passes through under water entanglement injector.In the operation, every meter nonwoven web width applies about 1200 water ejectors, and typically the current by the injector band are about 150 liters/minute or about 0.12 liter/minute water that flows through each the independent hole in the injector band.During water entanglement method, under the speed of the about 50 meters/min of about 10 meters/min-, nonwoven web passes through under water entanglement injector.Fabric speed can be conditioned so that change the degree that water tangles and handles.During water entanglement method, the temperature of water is about 30 ℃-40 ℃ and do not carry out processing such as the deionization or the demineralization of process water.The water entanglement process water of Shi Yonging is low inherently aspect metal ion content in these embodiments.In fact, the demineralization of the water that uses in the water entanglement procedure is made us expecting.

The detailed description of these methods is general and is applicable to the concrete pilot plant of the fabric that can be used for production following examples.It is restrictive that described condition is not intended to, and is used for illustrating the material described in the embodiment on the contrary and how can uses the supatex fabric equipment of other type that is different from concrete equipment used among the embodiment to produce.

Embodiment 1-prepares nonwoven web

According to aforesaid program, preparation comprises the nonwoven web that has with the bicomponent fiber of fan cake type (segmented pie) structure of 16 sections (segment).The component that the water of bicomponent fiber can not disperse is the PET polyester of F53HC grade, its logarithmic viscosity number is about 0.53 (EastmanChemical Company, Kingsport, TN, the U.S.) and with extruding as the dispersible sulfonic polyester of the water of second component.The dispersible sulfonic polyester called after of water SP05F, lot number TP06038931 (Eastman Chemical Company) and demonstrate the melt viscosities of about 3000 pools as measures in 240 ℃ and 1 radian per second shear rate.

Use is with the spinnerets in 2222 holes, under total rate of extrusion of passing through hole separately of about 0.6 gram/hole-min (ghm), polymer-extruded with two by fan cake type (segmented pie) bi-component spinning pack (Hills Inc., Melbourne FL), wherein the weight ratio of two polymer is 70 (PET): 30 (sulfonic polyesters).Use getter assembly stretching fused fiber extrudate and form the fiber that has about 9 microns average fibre diameter, has fan cake type (segmented pie) distribution of polymer of expectation.The multicomponent fibre of extruding is spread to be listed as on the forming belt to produce the nonwoven web that basic weight is 135 gram/square metre (gsm).

At room temperature strengthen the nonwoven web of embodiment 1 by compression between calender.During the method to surpass the estimated speed fusion drawn multicomponent fibre of about 5000m/min.When the nonwoven web of embodiment 1 when in baking oven, unrestrictedly nursing one's health for 120 ℃ because the stress relaxation of multicomponent fibre, in MD (vertically) and CD (laterally), nonwoven web is contracted to 60% * 57% of initial size respectively.

This nonwoven web has minimum inter-fibre-bond and produces the supatex fabric that water tangles as precursor by the processing subsequently of this nonwoven web of embodiment 1.

Embodiment 2

Use foregoing water entanglement unit, by means of high velocity water jets, the nonwoven web of water entanglement embodiment 1.During water entanglement method, fabric passes through machine with 40 meters/minute speed, and wherein nonwoven web stands two water under high pressure entanglement injectors with 150 crust hydraulic pressure runnings.First injector is applied to nonwoven web, when it is carried, so that the detailed catalogue pattern is applied to nonwoven web on 103 mesh sieve guipures.The second water entanglement injector is applied to the opposite side of described net, when its support is that the water entanglement drum of operation under the vacuum condition is gone up, so that obtain supatex fabric.

In the final step of water entanglement method, make wetting supatex fabric by drum dryer, wherein 70 ℃ of air pass through supatex fabric under the effect of the vacuum that keeps in 1.4 rice diameters drum.In the method, when in baking oven when heating supatex fabric only be half-dried and leave with wet condition.The measurement result of the time of staying of supatex fabric is about 5 seconds in baking oven.Along with supatex fabric is wound on the nuclear, some superfluous waters are extruded, and it is to be noted, water is muddy, owing to have the sulfonic polyester of emulsification, and formed sticking film, and when drying.Two observed results point out that some sulfonic polyesters are emulsified during this drying steps.

The energy that spends during water entanglement method is inversely proportional to the speed of the supatex fabric that passes through under injector, and wherein slower speed is converted into the water entanglement energy of the raising that is applied to supatex fabric.Similarly, the energy that is applied is directly proportional with the number of supatex fabric by the water entanglement injector platform under it, and wherein the square root of the water entanglement energy that applied of each injector platform and hydraulic pressure is in direct ratio.Use these relations, for the relative quantity of the water entanglement energy that relatively can estimate to be applied to nonwoven web.Under this situation of embodiment 2, the value that the water entanglement energy is distributed arbitrarily is 1.0, and wherein in embodiment subsequently, this value is applied to representative the increase with respect to the water entanglement energy of the method among the embodiment 2 of nonwoven web.

The basis weight of nonwoven fabrics that the water of embodiment 2 tangles is 139gsm (butt), and this is similar to the value of initial nonwoven web and shows does not have during water tangles or only few sulfonic polyester is removed.

In the environment temperature deionized water, wash the wetting supatex fabric 3 times of embodiment 2 and remove the sulfonic polyester of the aqueous phase emulsification of in supatex fabric, soaking into.After flushing and drying, reclaim soft supatex fabric.The supatex fabric that is reclaimed is very loose, demonstrates limited intensity, and because the bulk fibre on fabric face has the fine hair quality.Supatex fabric has the limited practicality as fabric.The loss in weight is 29% during rinsing step, and this shows from supatex fabric almost completely except that anhydrating dispersible sulfonic polyester.

This supatex fabric of embodiment 2 has the limited practicality as final products, but is made of the nonwoven web of microfiber, has wherein removed sulfonic polyester from multicomponent fibre and has exposed the PET microfiber.This precursor nonwoven fabric of embodiment 2 is further processed and makes the supatex fabric of subsequent embodiment 5 and 7.

Embodiment 3

Use foregoing water entanglement unit, by means of high velocity water jets, the nonwoven web of water entanglement embodiment 1.During water entanglement method, by this unit, wherein nonwoven web stands respectively four water under high pressure entanglement injectors with the expulsion pressures operation of 100 crust, 150 crust, 200 crust and 200 crust to nonwoven web with 10 meters/min speed.Preceding two injectors are applied to nonwoven web, when it is carried, so that the detailed catalogue pattern is applied to nonwoven web on 103 mesh sieve guipures.The third and fourth water entanglement injector is applied to the opposite side of nonwoven web, when its support is that the water entanglement drum of operation under the vacuum condition is gone up, so that produce supatex fabric.

In the final step of water entanglement method, make wetting supatex fabric by drum dryer, wherein 70 ℃ of air pass through supatex fabric under the effect of the vacuum that keeps in 1.4 rice diameters drum.In the method, when in baking oven when heating supatex fabric only be half-dried and leave with wet condition.The measurement result of the time of staying of supatex fabric is about 18 seconds in baking oven.Along with supatex fabric twines, some superfluous waters are extruded, and it is to be noted, water is muddy, owing to there is the sulfonic polyester of emulsification.When drying, on supatex fabric, the sulfonic polyester of emulsification has also formed sticking film.

The energy that spends during water entanglement method is inversely proportional to the speed of the supatex fabric that passes through under injector, and wherein slower speed is converted into the water entanglement energy of the raising that is applied to supatex fabric.Similarly, the energy that is applied is directly proportional with the number of supatex fabric by the water entanglement injector platform under it, and wherein the square root of the water entanglement energy that applied of each injector platform and hydraulic pressure is in direct ratio.Use these relations, in order to compare, calculating is with respect to the relative quantity of the water entanglement energy of this nonwoven web that is applied to embodiment 3 of embodiment 2.In this case, the water entanglement energy equals to distribute to the value of 8.3 times of a reference values of embodiment 2.The higher degree that water among the embodiment 3 tangles is because the number of employed water entanglement injector is 2 times, and 1/4 machining line speed, and this provides 4 times of time of staying under water entanglement injector.

The basis weight of nonwoven fabrics that the water of embodiment 3 tangles is 136gsm, this value and showing that is similar to the initial nonwoven web of embodiment 1 during water tangles, do not have or only the sulfonic polyester of minute quantity be removed.

In the environment temperature deionized water, wash the wetting supatex fabric 3 times of embodiment 3 and remove any sulfonic polyester of the aqueous phase emulsification of in supatex fabric, soaking into.After flushing and drying, reclaim soft supatex fabric.Observe about 28% the loss in weight, this shows from supatex fabric has removed whole basically sulfonic polyesters.This supatex fabric is very flexible, demonstrates good intensity, but has the fine hair surface texturisation, because loose surface fiber causes.This precursor web of embodiment 3 is used to further processing and makes the fabric of embodiment 6 and 9.

Embodiment 4

Use minimum water contact, the wetting supatex fabric that makes embodiment 2 is by foregoing water entanglement unit, so that remove sulfonic polyester from supatex fabric, and do not apply the entanglement of the multicomponent fibre in many extra fabrics.As pointed among the embodiment 2, find that sulfonic polyester in the supatex fabric is present in absorbed aqueous phase but not in the multicomponent fibre, and find that simple water flushing removed sulfonic polyester from supatex fabric.By the water unit that tangles, wherein supatex fabric stands the single water under high pressure entanglement injector operated to supatex fabric under 100 bar pressures with the speed of 50 meters/min.The temperature of water is about 20 ℃ during described method.

The fabric of embodiment 4 is dry and subsequently in the amount of 50 ℃ of washing calculates that the single water ejector of the method that is not implemented example 4 removes in deionized water in supatex fabric remaining sulfonic polyesters in environment temperature.Behind the supatex fabric of washing embodiment 4, only measure 3.0% loss in weight, this shows the sulfonic polyester of having removed the about 90wt% in the supatex fabric of embodiment 2 by this single water entanglement step.If single head is that temperature is higher effectively and for sulfonic polyester is removed for the body of removing the sulfonic polyester in the supatex fabric, preferably about 40 ℃-Yue 50 ℃, removing will be more effective.

Embodiment 5

Use foregoing water entanglement unit, the precursor nonwoven fabric of embodiment 2 is further carried out water with high velocity water jets and is tangled.。During this second water entanglement step subsequently, by water entanglement unit and make it stand four water under high pressure entanglement injectors, it is respectively with the expulsion pressures operation of 130 crust, 150 crust, 200 crust and 200 crust with the speed of 10 meters/min for the precursor nonwoven fabric that makes embodiment 2.Preceding two injectors are used to supatex fabric, when its when 61 mesh sieve guipures (available from Asten Johnson, Charleston SC) go up to be carried, so that sieve mesh pattern (meshpattern) is applied to supatex fabric.Third and fourth water entanglement injector is used to the opposite side of supatex fabric, when its water entanglement drum that is supported on operation under vacuum condition is gone up.

Use aforesaid relation, for relatively calculating relative quantity with respect to the water entanglement energy that in the method for embodiment 5, is applied to this supatex fabric of the method for embodiment 2.Water entanglement energy among the embodiment 5 equals to distribute to 8.5 times value of a reference value 1 of embodiment 2.The total water entanglement energy that is applied to supatex fabric in the method for the merging of embodiment 2 and 5 equals about 9.5 times value of the water entanglement energy that applies separately in the method for embodiment 2.This fabric demonstrates extraordinary fibre matting, and does not have bulk fibre from the teeth outwards.This fabric demonstrates good level and smooth surface texturisation.

Embodiment 6

Make water entanglement unit, the precursor nonwoven fabric of embodiment 3 is further carried out water with high velocity water jets and is tangled.During this second water entanglement step, make supatex fabric with the speed of 10 meters/min by the water unit that tangles, wherein make supatex fabric stand four water under high pressure entanglement injectors, it is respectively with the expulsion pressures operation of 130 crust, 150 crust, 200 crust and 200 crust.Preceding two injectors are used to the supatex fabric of embodiment 3, when it shifts on 61 mesh sieve guipures (available from AstenJohnson), so that sieve mesh pattern (mesh pattern) is applied to fabric.Third and fourth water entanglement injector is used to the opposite side of supatex fabric, when its water entanglement drum that is supported on operation under vacuum condition is gone up.

Use aforesaid relation, for relatively calculating relative quantity with respect to the water entanglement energy that in the method for embodiment 6, is applied to this supatex fabric of the method for embodiment 2.Water entanglement energy among the embodiment 6 equals to distribute to 8.5 times value of the arbitrary value of embodiment 2.The total water entanglement energy that is applied to supatex fabric in the method for the merging of embodiment 3 and 6 equals about 16.8 times value of the water entanglement energy that applies separately in the method for embodiment 2.

This fabric demonstrates extraordinary fibre matting, and does not have bulk fibre from the teeth outwards.This fabric demonstrates good level and smooth surface texturisation.

Embodiment 7

Make water entanglement unit, the precursor nonwoven fabric of embodiment 2 is further carried out water with high velocity water jets and is tangled.During this second water entanglement step, make supatex fabric with the speed of 10 meters/min by the water unit that tangles, wherein make supatex fabric stand four water under high pressure entanglement injectors, it is respectively with the expulsion pressures operation of 130 crust, 150 crust, 200 crust and 200 crust.Preceding two injectors are used to supatex fabric, when it is gone up when carrying at Formtec 14 (14 eye mesh screen) band (available from Albany International, Albany NY), so that scalping order pattern (coarsemesh pattern) is applied to supatex fabric.Difference between the fabric of the fabric of embodiment 5 and embodiment 7 is used forming belt, and wherein the basket weave outward appearance that the band among the embodiment 7 will be thicker gives fabric face, than the fabric of embodiment 5.Third and fourth water entanglement injector is used to the opposite side of supatex fabric, when its water entanglement drum that is supported on operation under vacuum condition is gone up.

Use aforesaid relation, for relatively calculating relative quantity with respect to the water entanglement energy that in the method for embodiment 7, is applied to this supatex fabric of the method for embodiment 2.Water entanglement energy among the embodiment 7 equals to distribute to 8.5 times value of the arbitrary value 1 of embodiment 2.The total water entanglement energy that is applied to supatex fabric in the method for the merging of embodiment 2 and 7 equals about 9.5 times value of the water entanglement energy that applies separately in the method for embodiment 2.

Embodiment 8

Reach 5 minutes conditioning time by pieces of fabric being placed on the constraint frame and forcing to nurse one's health supatex fabric in the air-oven, make the supatex fabric heat setting of embodiment 5 at 130 ℃.The constraint frame is 14 inches * 14 inches having around the frame of the pin of frame periphery, separates with 1/2 inch spacing between pin.The effect of contraction of pin prevents the contraction of supatex fabric when heating.Conditioning under heating up causes the stress relaxation in the fiber.

Embodiment 9

Reach 5 minutes conditioning time by non-woven fabric sheet being placed on the constraint frame and forcing to nurse one's health supatex fabric in the air-oven, make the fabric heat setting of embodiment 6 at 130 ℃.The constraint frame is 14 inches * 14 inches having around the frame of the pin of frame periphery, separates with 1/2 inch spacing between pin.The effect of contraction of pin prevents the contraction of supatex fabric when heating.Conditioning under heating up causes the stress relaxation in the fiber.

Embodiment 10

Reach 5 minutes conditioning time by non-woven fabric sheet being placed on the constraint frame and forcing to nurse one's health supatex fabric in the air-oven, make the fabric heat setting of embodiment 7 at 130 ℃.The constraint frame is 14 inches * 14 inches having around the frame of the pin of frame periphery, separates with 1/2 inch spacing between pin.The effect of contraction of pin prevents the contraction of supatex fabric when heating.Conditioning under heating up causes the stress relaxation in the fiber.

Comparative Examples 1

Use foregoing water entanglement unit, the fabric of embodiment 1 carries out water with high velocity water jets and tangles.During water entanglement method, make fabric pass through machine with the speed of 10 meters/min, wherein make nonwoven web stand four water under high pressure entanglement injectors, it is operated with the expulsion pressure of 100 crust, 150 crust, 200 crust and 200 crust respectively.Preceding two injectors are used to fabric, when it shifts on 103 mesh sieve guipures, so that the detailed catalogue pattern is applied to fabric.Third and fourth opposite side that water entanglement injector is used to net is when its water entanglement drum that is supported on operation under vacuum condition is gone up.

In the final step of water entanglement method, make wet fabric pass through drum dryer, wherein 70 ℃ of air pass through fabric under the effect of the vacuum that keeps in 1.4 rice diameters drum.In the method, fabric is only half-dried, when heating in baking oven, and leaves with wet condition.The measurement result of the time of staying of fabric in baking oven is about 18 seconds.Along with fabric is wound on the nuclear, some superfluous waters are extruded, and it is to be noted, water is muddy, show the sulfonic polyester of some emulsifications.

The fabric that forms by this water entanglement step in deionized water at 45 ℃ and in the family expenses washing machine, use hot water (48 ℃) circulation to wash.Fabric has the outward appearance of height wrinkle, and wherein many bulk fibres from the teeth outwards.Fabric is very " sticking (tacky) " or " sticking (clingy) ", this be since in fabric the loose person's character of surface fiber, and for textile application, do not make us expecting.

Comparative Examples 2

Reach 5 minutes conditioning time by pieces of fabric being placed on the constraint frame and forcing to nurse one's health supatex fabric in the air-oven, make the supatex fabric heat setting of Comparative Examples 1 at 130 ℃.The constraint frame is 14 inches * 14 inches having around the frame of the pin of frame periphery, separates with 1/2 inch spacing between pin.The effect of contraction of pin prevents the contraction of supatex fabric when heating.Conditioning under heating up causes the stress relaxation in the fiber.

This fabric demonstrates bulk fibre from the teeth outwards and has " sticking (tacky) " or " sticking (clingy) " feel, because excessive bulk fibre from the teeth outwards.

Claims

1. method that is used to make supatex fabric, it comprises:

(A) collect multicomponent fibre to form nonwoven web; Wherein said multicomponent fibre comprises the polymer that dispersible sulfonic polyester of at least a water and at least a water can not disperse; Wherein said multicomponent fibre has a plurality of territories, and described territory comprises the polymer that described water can not disperse; Wherein said territory is isolated from each other basically by the dispersible sulfonic polyester of described water between described territory;

(B) described nonwoven web is contacted with water and remove a part the dispersible sulfonic polyester of described water, form microfiber webs thus; With

(C) water tangles described microfiber webs to produce described supatex fabric.

2. according to the process of claim 1 wherein that described sulfonic polyester comprises dicarboxylic acid monomer's residue, sulfomonomer residue, diol monomer residue and repetitive.

3. according to the method for claim 2, wherein said dicarboxylic acids is selected from aliphatic diacid, cycloaliphatic dicarboxylic acid, aromatic dicarboxylic acid and its combination.

4. according to the method for claim 3, wherein said dicarboxylic acids is selected from butanedioic acid, glutaric acid, adipic acid, azelaic acid, decanedioic acid, fumaric acid, maleic acid, itaconic acid, 1,3-cyclohexane dicarboxylic acid, 1,4-cyclohexane dicarboxylic acid, diglycolic acid, 2,5-norcamphane dicarboxylic acids, phthalic acid, terephthalic acid (TPA), 1,4-naphthalene dicarboxylic acids, 2,5-naphthalene dicarboxylic acids, 2,6-naphthalene dicarboxylic acids, 2,7-naphthalene dicarboxylic acids, diphenic acid, 4,4 '-oxydiphenyl formic acid (oxydibenzoic), 4,4 '-sulfonyldibenzoic acid, M-phthalic acid and its combination.

5. according to the method for claim 2, wherein said sulfomonomer is the metal sulfonate of sulfosalicylic phthalate, sulfo group terephthalic acid (TPA), sulfoisophthalic acid or its combination.

6. according to the method for claim 2, wherein said glycol residue is selected from ethylene glycol, diethylene glycol (DEG), triethylene glycol, polyethylene glycol, 1, ammediol, 2,4-dimethyl-2-ethyl hexane-1,3-glycol, 2,2-dimethyl-1, ammediol, 2-ethyl-2-butyl-1, ammediol, 2-ethyl-2-isobutyl group-1, ammediol, 1, the 3-butanediol, 1, the 4-butanediol, 1, the 5-pentanediol, 1, the 6-hexylene glycol, 2,2,4-trimethyl-1, the 6-hexylene glycol, thiodiethanol, 1, the 2-cyclohexanedimethanol, 1, the 3-cyclohexanedimethanol, 1, the 4-cyclohexanedimethanol, 2,2,4,4-tetramethyl-1, the 3-cyclobutanediol, terephthalyl alcohol (xylylenediol) and its combination.

7. according to the method for claim 2, wherein said sulfonic polyester further comprises at least a branched monomer.

8. according to the method for claim 7, wherein said branched monomer is at least aly to be selected from 1,1,1-trimethylolpropane, 1,1,1-trimethylolethane, glycerine, pentaerythrite, erythrite, threitol, dipentaerythritol, D-sorbite, trimellitic anhydride, pyromellitic acid dianhydride, dihydromethyl propionic acid or its combination.

9. according to the process of claim 1 wherein that the polymer that described water can not disperse is selected from polyene footpath, polyester, polyamide, polyactide, polycaprolactone, Merlon, polyurethane, polyvinyl chloride and its combination.

10. according to the process of claim 1 wherein that the shaping section of described multicomponent fibre is fabric of island-in-sea type, fan cake type or core-skin type configuration.

11. according to the process of claim 1 wherein that described sulfonic polyester has at least 57 ℃ glass transition temperature (Tg) and the dispersible sulfonic polyester of described water comprises

(i) residue of one or more dicarboxylic acids;

The about 40mol% of (ii) about 4-, based on total repetition unit, the residue of at least a sulfomonomer, one or more sulfonate group that it has 2 functional groups and is attached to aromatics or cyclic aliphatic ring, wherein said functional group is hydroxyl, carboxyl or its combination;

H-(OCH ₂-CH ₂) _n-OH

Wherein n is the integer of 2-about 500; With

The (iv) about 25mol% of 0-, based on total repetition unit, have 3 or the residue of the branched monomer of above functional group, wherein said functional group is hydroxyl, carboxyl or its combination;

Wherein said fiber has a plurality of section of the polymer that described water can not disperse and described sections of comprising and is isolated from each other basically by the described sulfonic polyester between described section.

12. according to the process of claim 1 wherein that described sulfonic polyester has the melt viscosity less than 12,000 pools, it is measured in 240 ℃ and 1 radian per second shear rate.

13. according to the method for claim 12, wherein said sulfonic polyester has the melt viscosity less than 6,000 pools, it is measured in 240 ℃ and 1 radian per second shear rate.

14. according to the method for claim 13, wherein said sulfonic polyester has the melt viscosity less than 4,000 pools, it is measured in 240 ℃ and 1 radian per second shear rate.

15. according to the process of claim 1 wherein that described collection is selected from the method that mechanical sewing, chemical bonding, hot calendering, ultrasonic fusion and water tangles and finishes by at least a.

16. according to the method for claim 15, wherein said collection is tangled by water and is finished and water entanglement energy in described water entanglement step relates to about 20%-about 50% of the amount of the water entanglement energy that is spent in the step (C).

17. according to the process of claim 1 wherein that described multicomponent fibre is by spunbond method or meltblowing method production.

18. according to the process of claim 1 wherein that the weight of described nonwoven web is about 10 gram/m ²-Yue 800 gram/m ²

19. according to the method for claim 18, the weight of wherein said nonwoven web is about 10 gram/m ²-Yue 400 gram/m ²

20. according to the method for claim 19, the weight of wherein said nonwoven web is about 50 gram/m ²-Yue 150 gram/m ²

21. according to the process of claim 1 wherein that the extraction temperature of the dispersible sulfonic polyester of described water is about 20 ℃-Yue 100 ℃.

22. according to the process of claim 1 wherein that the pressure of water is about 30 Ba-Yue 600 crust during step (B).

23. according to the method for claim 22, wherein the pressure of water is the about 300barr of about 50barr-during step (B).

24. contact the time that reaches the about 100wt% of about 30wt%-that is enough to remove the dispersible sulfonic polyester of whole water contained in the described nonwoven web with water at nonwoven web described in the step (B) according to the process of claim 1 wherein.

25., wherein contact the time that is enough to from described nonwoven web, remove the dispersible sulfonic polyester of whole water that reaches with water greater than 90wt% at nonwoven web described in the step (B) according to the method for claim 24.

26., wherein contact the time that is enough to from described nonwoven web, remove the dispersible sulfonic polyester of whole water that reaches with water greater than 95wt% at nonwoven web described in the step (B) according to the method for claim 25.

27. according to the process of claim 1 wherein that described nonwoven web contacts the about 600 seconds time of about 10-that reaches with water, the dispersible sulfonic polyester of described whereby water is dispersed or is dissolved.

28. according to the process of claim 1 wherein that microfiber in the microfiber webs has the average fineness less than the dawn number of 30% described multicomponent fibre.

29. according to the method for claim 28, wherein the described microfiber in described microfiber webs has 1dpf or littler average fineness.

30. according to the method for claim 29, wherein the described microfiber in described microfiber webs has 0.5dpf or littler average fineness.

31., contact with water at nonwoven web described in the step (B) according to the process of claim 1 wherein the use water ejector.

32., wherein use 1-8 sprinkler head according to the method for claim 31.

33. according to the method for claim 31, wherein the amount of used water is about 500 times to about 1000 times of weight of described nonwoven web in the step (B).

34. according to the process of claim 1 wherein that the washings from step (B) and step (C) can be recovered.

35. according to the method for claim 34, wherein 80% or more washings be recovered.

36. according to the process of claim 1 wherein that the temperature of the water in the step (C) is less than 40 ℃.

37. according to the process of claim 1 wherein that the pressure of the water in the step (C) is about 150 Ba-Yue 250 crust.

38. according to the process of claim 1 wherein that the dispersible sulfonic polyester of water less than in the step (C) of 1wt% removes from described microfiber webs.

39., wherein in step (C), remove from microfiber webs less than the dispersible sulfonic polyester of the water of 0.5wt% according to the method for claim 38.

40., wherein in step (C), remove from microfiber webs less than the dispersible sulfonic polyester of the water of 0.1wt% according to the method for claim 38.

41. undertaken by sprinkler head according to the process of claim 1 wherein that described water in the step (C) tangles.

42. according to the method for claim 41, wherein the number of sprinkler head is 1-about 20.

43. a method that is used to make supatex fabric, it comprises:

(A) collect multicomponent fibre to form nonwoven web; Wherein said multicomponent fibre comprises the polymer that dispersible sulfonic polyester of at least a water and at least a water can not disperse; Wherein said multicomponent fibre has a plurality of territories, and described territory comprises the polymer that described water can not disperse; Wherein said territory is isolated from each other basically by the dispersible sulfonic polyester of described water between described territory; With

(B) described nonwoven web is contacted with water and remove the described sulfonic polyester of a part, form microfiber thus, and simultaneously water tangles described microfiber to produce described supatex fabric.

44. according to the method for claim 43, wherein said sulfonic polyester comprises dicarboxylic acid monomer's residue, sulfomonomer residue, diol monomer residue and repetitive.

45. according to the method for claim 44, wherein said dicarboxylic acids is selected from aliphatic diacid, cycloaliphatic dicarboxylic acid, aromatic dicarboxylic acid and its combination.

46. method according to claim 45, wherein said dicarboxylic acids is selected from butanedioic acid, glutaric acid, adipic acid, azelaic acid, decanedioic acid, fumaric acid, maleic acid, itaconic acid, 1,3-cyclohexane dicarboxylic acid, 1,4-cyclohexane dicarboxylic acid, diglycolic acid, 2,5-norcamphane dicarboxylic acids, phthalic acid, terephthalic acid (TPA), 1,4-naphthalene dicarboxylic acids, 2,5-naphthalene dicarboxylic acids, 2,6-naphthalene dicarboxylic acids, 2,7-naphthalene dicarboxylic acids, diphenic acid, 4,4 '-oxydiphenyl formic acid (oxydibenzoic), 4,4 '-sulfonyldibenzoic acid, M-phthalic acid and its combination.

47. according to the method for claim 44, wherein said sulfomonomer is the metal sulfonate of sulfosalicylic phthalate, sulfo group terephthalic acid (TPA), sulfoisophthalic acid or its combination.

48. method according to claim 44, wherein said glycol residue is selected from ethylene glycol, diethylene glycol (DEG), triethylene glycol, polyethylene glycol, 1, ammediol, 2,4-dimethyl-2-ethyl hexane-1,3-glycol, 2,2-dimethyl-1, ammediol, 2-ethyl-2-butyl-1, ammediol, 2-ethyl-2-isobutyl group-1, ammediol, 1, the 3-butanediol, 1, the 4-butanediol, 1, the 5-pentanediol, 1, the 6-hexylene glycol, 2,2,4-trimethyl-1, the 6-hexylene glycol, thiodiethanol, 1, the 2-cyclohexanedimethanol, 1, the 3-cyclohexanedimethanol, 1, the 4-cyclohexanedimethanol, 2,2,4,4-tetramethyl-1, the 3-cyclobutanediol, terephthalyl alcohol (xylylenediol) and its combination.

49. according to the method for claim 44, wherein said sulfonic polyester further comprises at least a branched monomer.

50. method according to claim 49, wherein said branched monomer is at least aly to be selected from 1,1,1-trimethylolpropane, 1,1,1-trimethylolethane, glycerine, pentaerythrite, erythrite, threitol, dipentaerythritol, D-sorbite, trimellitic anhydride, pyromellitic acid dianhydride, dihydromethyl propionic acid or its combination.

51. according to the method for claim 43, the polymer that wherein said water can not disperse is selected from polyene footpath, polyester, polyamide, polyactide, polycaprolactone, Merlon, polyurethane, polyvinyl chloride and its combination.

52. according to the method for claim 43, the shaping section of wherein said multicomponent fibre is fabric of island-in-sea type, fan cake type or core-skin type configuration.

53. according to the method for claim 43, wherein said sulfonic polyester has at least 57 ℃ glass transition temperature (Tg) and the dispersible sulfonic polyester of described water and comprises:

(i) residue of one or more dicarboxylic acids;

H-(OCH ₂-CH ₂) _n-OH

Wherein n is the integer of 2-about 500; With

54. according to the method for claim 43, wherein said sulfonic polyester has the melt viscosity less than 12,000 pools, it is measured in 240 ℃ and 1 radian per second shear rate.

55. according to the method for claim 54, wherein said sulfonic polyester has the melt viscosity less than 6,000 pools, it is measured in 240 ℃ and 1 radian per second shear rate.

56. according to the method for claim 56, wherein said sulfonic polyester has the melt viscosity less than 4,000 pools, it is measured in 240 ℃ and 1 radian per second shear rate.

57. according to the method for claim 43, wherein said collection is finished by at least a method that is selected from mechanical sewing, chemical bonding, hot calendering, ultrasonic fusion and water entanglement.

58. according to the method for claim 57, wherein said collection is tangled by water and is finished and water entanglement energy in described water entanglement step relates to about 20%-about 50% of the amount of the water entanglement energy that is spent in the step (C).

59. according to the method for claim 43, wherein said multicomponent fibre is produced by spunbond method or meltblowing method.

60. according to the method for claim 43, the weight of wherein said nonwoven web is about 10 gram/m ²-Yue 800 gram/m ²

61. according to the method for claim 60, the weight of wherein said nonwoven web is about 10 gram/m ²-Yue 400 gram/m ²

62. according to the method for claim 61, the weight of wherein said nonwoven web is about 50 gram/m ²-Yue 150 gram/m ²

63. according to the method for claim 43, the extraction temperature of the dispersible sulfonic polyester of wherein said water is about 20 ℃-Yue 100 ℃.

64. according to the method for claim 43, wherein the pressure of water is about 30 Ba-Yue 600 crust during step (B).

65. according to the method for claim 64, wherein the pressure of water is the about 300barr of about 50barr-during step (B).

66., wherein contact the time that reaches the about 100wt% of about 30wt%-that is enough to remove the dispersible sulfonic polyester of whole water contained in the described nonwoven web with water at nonwoven web described in the step (B) according to the method for claim 43.

67., wherein contact the time that is enough to from described nonwoven web, remove the dispersible sulfonic polyester of whole water that reaches with water greater than 90wt% at nonwoven web described in the step (B) according to the method for claim 66.

68., wherein contact the time that is enough to from described nonwoven web, remove the dispersible sulfonic polyester of whole water that reaches with water greater than 95wt% at nonwoven web described in the step (B) according to the method for claim 67.

69. according to the method for claim 43, wherein said nonwoven web contacts the about 600 seconds time of about 10-that reaches with water, the dispersible sulfonic polyester of described whereby water is dispersed or is dissolved.

70. according to the method for claim 43, wherein the microfiber in the microfiber webs has the average fineness less than the dawn number of 30% described multicomponent fibre.

71. according to the method for claim 70, wherein the described microfiber in described microfiber webs has 1dpf or littler average fineness.

72. according to the method for claim 71, wherein the described microfiber in described microfiber webs has 0.5dpf or littler average fineness.

73. according to the method for claim 43, wherein use water ejector, contact with water at nonwoven web described in the step (B).

74., wherein use 1-8 sprinkler head according to the method for claim 73.

75. according to the method for claim 73, wherein the amount of used water is about 500 times to about 1000 times of weight of described nonwoven web in the step (B).

76. according to the method for claim 43, wherein the washings from step (B) and step (C) can be recovered.

77. according to the method for claim 76, wherein 80% or more washings be recovered.

78. according to the method for claim 43, wherein the temperature of the water in the step (C) is less than 40 ℃.

79. according to the method for claim 43, wherein the pressure of the water in the step (C) is about 150 Ba-Yue 250 crust.

80., wherein remove from described microfiber webs less than the dispersible sulfonic polyester of water in the step (C) of 1wt% according to the method for claim 43.

81. 0 method is wherein removed from microfiber webs less than the dispersible sulfonic polyester of the water of 0.5wt% in step (C) according to Claim 8.

82. 1 method is wherein removed from microfiber webs less than the dispersible sulfonic polyester of the water of 0.1wt% in step (C) according to Claim 8.

83. according to the method for claim 43, wherein the described water in the step (C) tangles and is undertaken by sprinkler head.

84. 3 method according to Claim 8, wherein the number of sprinkler head is 1-about 20.

85. according to the method for claim 1 or 43, wherein said supatex fabric is heat setting.

86. by the supatex fabric that the method for claim 1 or claim 43 is produced, wherein said supatex fabric is used at least a of following terminal use: clothes, curtain, upholstery, uniform, personal care product, hospital/surgery and other medical disposable product, multi-layer nonwoven cloth, laminated thing and compound, protection fabric and layer, geotextile, industrial wipes and filter medium.