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Publication numberUS2938811 A
Publication typeGrant
Publication dateMay 31, 1960
Filing dateNov 9, 1959
Priority dateNov 9, 1959
Publication numberUS 2938811 A, US 2938811A, US-A-2938811, US2938811 A, US2938811A
InventorsHermes Julius
Original AssigneeMartin Proc Company Inc
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Method of conditioning polyester textile material and the resulting products
US 2938811 A
Abstract  available in
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Claims  available in
Description  (OCR text may contain errors)

United States Patent METHOD OF CONDITIONING POLYESTER TEX.

TILE MATERIAL AND THE RESULTING PROD- UCTS Julius Hermes, Martinsville, Va., assignor to Martin Processing Company, Incorporated, Martinsvrlle, Va., a corporation of Virginia N0 Drawing. Filed Nov. 9, 1959, Ser. No. 851,506

5 Claims. (Cl. 117102) This invention relates to the treatment of synthetic textile material of the kind known as Dacron which, as is well known in the art, is a condensation polymer of terephthalic acid and ethylene glycol, also known as polyethylene terephthalate or, perhaps more familiarly, as polyester material. More particularly, the invention relates to a procedure for conditioning such material whereby it is given substantially new and different properties rendering it especially adaptable to subsequent processing. The invention also relates to the resulting products, and especially to the undyed products resulting from the conditioning treatment. Reference to synthetic textile material or polyester material hereinafter is to be regarded for the sake of brevity as referring solely to the aforesaid synthetic textile material unless indicated otherwise by the context.

The method of this invention comprises subjecting the polyester material to heating at a very high temperature using a hot liquid medium for efiecting the heating. The importance of this type of heating is the liquid or wet, as distinguished from the conventional dry form of heat: ing, such as on drying cans or the like. The liquid heat treatment effects an actual impregnation of the polyester textile material with the hot liquid that imparts to the treated material new properties, eg anti-pilling properties, not obtainable by dry heating, and likewise condi tions the polyester material for more effective additional treatments such as, for example, dyeing. This liquid heat treatment or conditioning of the polyester material is preferably carried out without supplemental treatment thereof except for removal or substantial removal of the ice form surface. It appears that the pills or ballsformed' on the polyester fiber materials do not'break or fall off because of the increased strength and perhaps other char-, acteristics of these fibers different from the natural fibers.

This polling problem has become acute in view of the fact that the polyester fiber fabrics and garments of the kind mentioned above exhibit this undesirable surface etfect after relatively short periods of wear or Washing. In suiting materials, the pilling eifect shows up mainly on collars, cuffs, sleeves and other portions of the garments that normally rub against each other or against other surfaces during wear of the garment, and as a result of this abrasion, even though slight, numerous pills or balls form on the surface. This undesirable effect is especially noticeable and pronounced in'knitted wear,

heating liquid. Alternatively, this liquid heat treatment may be carried out first and then followed by additional treatments of the polyester material such as dyeing, since the polyester material is thereby rendered especially amenable to dyeing.

This subsequent treatment of the polyester textile material, however, is not required and is used only when and as desired to produce some additional characteristic, such as, for example, dyeing of the material. Independently of dyeing or other subsequent operation, the polyester material treated with the highly heated liquid in accord ance with the present invention acquires new physical properties, such as the above mentioned anti-pilling property.

The anti-pilling property is especially important. It has been found that fabrics or garments made from the foregoing polyester textile fibers or mixtures thereof with other fibers, when subjected to abrasion such as is ordinarily encountered in wearing or laundering, will produce pills or small balls of the abraded fibers that do not fall off or become separated from the fabric, but adhere to it and produce a very unattractive surface appearance. This effect is in contrast to the abrasion effects experienced with wool and other natural fibers, and in which pills or balls either do not form on the surface of the goods or if they do form they break oft, leaving a smooth uni- 1 such as. sweaters made of Dacron. The numerous pills formed on the surface of the sweaters adhere so tenaciously that they cannot be removed by the usual bI'HSh'.

I have discovered, in accordance with the present in vention, that this important commercial problem can be effectively solved by a heat treatment of these synthetic polyester fiber fabrics with a highly heated liquid. a result of this heat treatment, the fabric shows littleor no tendency to produce pills or balls even under severe abrasion. In a commercially advantageous example of the process of my invention, I subject the polyester fiber fabricl'to an impregnation treatment with a highly heated, non} aqueous, non-evaporative liquid that quickly heats the polyester textile material to the temperature of the liquid and effects rapid penetration thereof by this liquid. In fact, the penetration is sufiiciently deep and uniform that a small amount of the treating liquid remains imbedded in the fibers of the fabric even after thorough washing and drying of the fabric. This small residual impregnant in the fabric aids in identifying the polyester textile material that has the non-pilling characteristic established therein by treatment of the fabric at a high temperature with the highly heated liquid in accordance with th present invention, and also confers other desirableprop erties such as those of an internal lubricant'which enables garment manufacturers more readily and conveniently to process these fabrics during the garment manufacturing operations. For example, in cutting to pattern numerous layers of stacked polyester fabrics that have been treated in accordance with the present invention, the residual impregnant greatly facilitates the cut ting operation by helping to keep the cutting knife cool. For carrying out the process of my invention, 1 have found that it is important to utilize as the highly heated liquid medium, a liquid having a high boiling point sub: stantially above the boiling point of water, e.g. about 250 F or higher, there being no upper limit on the boiling point which in practice may run as'high as about 550 F. with certain high boilingliquidsfi I Another important characteristic of the liquid tobe used in my process is that it should be non-evaporative, like glycerine and other polyhydric alcohols, as distinct from the evaporative or vaporizable lower aliphatic alcohols or ethers. I 1

A further important aspect of the heated liquid medium used in my invention is that it should be anhydrous or free of water so as to maintain the desired high boiling point of the liquid medium and to avoid bubbling and evaporation of the liquid which would otherwise occur in Suitable, but non-limiting, examples of'liquids for -use in my invention are polyhydroxy compounds such' as ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, butylene glycol and glycerine. 'Of the foregoing, the glycols and glycol ethers or polyglycols are. preferred. In viewofthe fact that the etfectiveness of'thel highly heated solvent apparently does not. depend upon any of its chemical properties, but instead uponits physical'properties, particularly the high boiling point.

.therefore easily removable or substantially removable from the polyester textile material after treatment. Due to,its vsomewhat higher boiling point, and consequently lower vapor pressure at a given elevated temperatureof treatment, the dipropylene. glycol ofiers unusually attractive properties for'commercial use.

These and similar non-aqueous, non-evaporative high boiling liquids will, When highly heated, penetrate and impregnate the polyester textile material to impart to it anti-pilling or other new and vdesirable properties and to facilitate subsequent additional treatment such as dyeing'thereof. By using this highly heated liquid for conditioning the polyester textile material before application of the dyestuff, the fibers of the polyester textile material are made markedly receptive to penetration and impreg nation by the dyestutf. When the polyester textile inaterial is first conditioned in this, manner, the subsequent dyeing operation can be carried out in a markedly shorter time thanis normally required. I At the present time it is very difficnlt to dye polyester materials. have been designed to increase the boiling point of water, thus causing the dyestutf to penetrate more readily into the polyester fibers. This pressure equipment is very costly and is by no means the answer to efiicient dyeing procedures. Another method that has been proposed for increasing the dye absorption of the polyester material is dyeing on conventional equipment'using carriers n the dyebath. The most eflective carriers are phenollc compounds. These phenols'have several .dis-

Various types of high pressure equipment advantages such as that they affect the light fastness adversely, are very difficult to remove from the polyester material, and increase the dyeing cost considerably. An illustration of the dyeing problems encountered when polyester materials are dyed by conventional methods is thatv one large textile concern currently has a fully pressurized dye plant under construction solely for the dyeing of polyester materials. The dyeing cycle for polyester materials on conventional equipment is approximately 78-14 hours, depending on the depth of shade desired.

The polyester'material conditioned in accordance with the present invention may *be dyed very readilyon con.- ventional dyeing equipment without the use of carriers or high pressure equipment. The full dyeing cycle is less than3 hours and complete dyestuff exhaustion is achieved at comparatively low temperatures. It has been found that complete dye exhaustion takes place at temperatures as low as 180 F.

. Another important characteristic:of the heatedorganic material in a simple manner such as by washing with 1- water, while 'still leaving a relatively small amount entrapped inthe fiber structure;

Further, the liquid heating medium should preferably be neutral in character, neither strongly acid nor strongly basic, and otherwise substantially inert to the polyester textile material to avoid any adverse effects when the polyester textile material is impregnated with the hot liquid.

Regardingtheform of polyester textile material that may be treated in accordance with the processof my invention, this process has been found to be applicable to practically any and all forms, such as filaments, staple fibers, threads, yarns andwoven or knitted goods.

The optimum operating temperature for heat treatment of the fabric or other polyester textile material will vary with the particular fiber, and particularly its resistance to heat. For example, when treating Dacron in the form of fabrics, the temperature should not go substantially above 365 F. with one kind of Dacron, namely Dacron type 64, although with another type of Dacron, namely type 54, a temperature of about 385 F. is advantageously employed. In general, the organic liquids, used should have a boiling point within the range of about 250 F. to 550 F., and preferably about 350 to 550 F.; should not harm the fabric or other polyester material; and should be removable or substantially removable therefrom after the heat treatment has been completed. I

Where it is desired to effect dyeing subsequently to the wet heat treating process of this invention, practically any and all known types of dyestuffs suitable for the textile materials undergoing treatment may be used. These include vats, Indigosols, basic dyes, acid dyes and dispersed dyes, as well as dyestufis more recently developed for dyeing some of the newer synthetic fibers, such as, for example, Latyl dyes, which are also dispersed dyes.

Regarding the equipment necessary for carrying out this new polyester textile material conditioning method, it isnot critical in character and is subject to wide variations. The essential requirements are a suitable container for heating the non-aqueous, non-evaporative liquid treating agent to the desired higher temperatures.

The following are illustrative but non-limiting examples of the process of my invention, in which synthetic polyester fiber textile materials are treated at high temperatures to prevent or minimizepilling effects and to impartthereto other improved properties such as better dye receptivity.

' Example 1 A clean, dry, Dacron fabric is passed through a bath of diethylene glycol heated to a'temperature of approximately 360-365 F; I have found'that the effectiveness of this'treatment can be obtained almost immediately,

that is, with'about ten seconds treatment of the cloth in this highly heated diethylene glycol bath. After the Dacron fabric passes through this liquid bath, the surplus diethylene glycol is squeezed off by squeeze rolls or the like and the treated cloth is then passed through a-water bath at iordinary room temperature which removes substantially all of;the diethylene glycol but leaves a 'very small amount of the diethylene glycol entrapped'in the Dacron fibers. After washing with water, the polyester fabricis dried and may be used as such or it' may be'dyedor otherwise finished'as desired. If it is to be 'dyed immediately following the conditioning step, then of course it need not first be dried.

In the event other similar non-aqueous, non-evaporative, water-soluble liquids such as those mentioned above are used for effecting the conditioning treatment, then the procedure described in Examplejl abovewould be gen.-

erally followed with any necessary adjustments of the temperature for the specific treating liquid, although in 7 general the temperatures wouldbe of the same-high order and sufficient to etfect-atleast afpartial penetration of the polyester textile'fiber fabric with the highly heated treating liquid, as a result of which the fabric will not thereafter show the usual pilling effect upon abrasion.

Generally speaking, the residual treating liquid retained in and carried by the polyester textile material, even after washing and drying, will be relatively small such as of the order of about 2% by weight.

It has been found that the process of my invention may be applied satisfactorily, as above described, to cloth or the like consisting of a single type of Dacron polyester fibers, or composed of a mixture of Dacron and other fabrics, such as, for example, Dacron and wool, etc., and a subsequent uniform or union dyeing result obtained, assuming of course the proper selection of dyestuff or dyestuifs suited for dyeing the respective fibers.

Example 2 A number of skeins of Dacron polyester tow were treated as follows: skeins Nos. 1, 2 and 3 were Dacron type 54 and one-half of each skein was immersed for 15 seconds in diproplyene glycol at a temperature of 385 F. Skeins Nos. 4 and were Dacron type 64 and one-half of each skein was treated for seconds in dipropylene glycol at a temperature of 365 F., it being possible to treat the type 64 product at a somewhat lower temperature. a

After treating the Dacron skeins in dipropylene glycol in the foregoing fashion, the treated skeins were chilled in cold water for the purpose of suddenly closing the fiber pores and thereby entrapping relatively small traces of dipropylene glycol in the fiber. The skeins were then washed in warm water and subjected to dyeing in an otherwise conventional manner without the use of carrier or high pressure equipment, i.e., in substantially the same manner as in the conventional dyeing of acetate-rayon. In each case the dyestuff was pasted with a small amount of Alkanol HCS (du Pont) which acts as a dispersing agent for the dyestuif.

All dyeings were carried out in an aqueous medium at a temperature of 200 F. for a period of one-half hour. The dyestuffs employed were as follows:

Skein No. 1-Acetamine Rubine B (du Pont) Skein No. 2Eastman Blue BNN (Tennessee-Eastman) Skein No. 3Acetamine Fast Yellow 4 RL (du Pont) Skein No. 4Latyl Brilliant Blue 26 (du Pont) Skein No. 5Sevron Blue 56 (du Pont) The first four dyestuffs are dispersed dyestuffs, while the last dyestuff is a cationic dyestufi.

In all cases the conditioned Dacron (i.e., the half of the skein that had been immersed in the heated dipropylene glycol) dyed darker and more evently than non-conditioned Dacron.

The process as described in the specification and defined in the claims herein for quickly heating the polyester textile material of the kind indicated above with an anhydrous organic liquid at a temperature between approximately 250 and 550 F., but preferably between about 350 and 550 F., but below the softening or damaging point for the polyester textile material, requires a relatively very short time, e.g. less than about one minute and usually in the order of eight to fifteen seconds time as specified in the illustrative but non-limiting examples herein.

This application is a continuation-in-part of my prior application Serial No. 491,173, filed February 28, 1955, now abandoned, which in turn is a continuation-in-part of my prior application Serial No. 415,155, filed March 9, 1954, now abandoned.

The above described materials, conditions and procedures are subject to modifications and variations, as indicated in the appended claims.

What is claimed is:

l. A process of improving the dyeability and minimizing the pilling effects in a synthetic polyester textile material comprising a condensation polymer of terephthalic acid and ethylene glycol, comprising the steps of immersing the textile material in a heated, anhydrous, relatively high-boiling, water-soluble, inert, organic liquid medium in the substantial absence of any dyestuflf and at an elevated temperature ofat least 250 F. but below the softening point of the textile material, for a period of time sufiicient to effect impregnation of the textile material with the heated organic liquid medium and to modify the fiber structure of the textile material by penetration of said organic liquid medium into said fiber structure but without otherwise affecting the fiber structure, removing the textile material from the heated organic liquid medium, and immediately thereafter contacting the textile material with relatively cool water, thereby substantially removing the adhering organic liquid medium from the textile material while leaving entrapped within the fiber structure thereof a small residual amount of said organic liquid medium.

2. A process as defined in claim 1 in which the organic liquid medium is at an elevated temperature of at least 350 F.

3. A product as prepared by the process of claim 1.

4. A process of improving the dyeability and minimizing the pilling efiects in a synthetic polyester textile material comprising a condensation polymer of terephthalic acid and ethylene glycol, comprising the steps of immersing the textile material in a heated, anhydrous, relatively high-boiling, water-soluble, inert, organic liquid medium consisting essentially of a polyhydric alcohol selected from the group consisting of ethylene glycol, di ethylene glycol, propylene glycol, dipropylene glycol, butylene glycol, and glycerine in the substantial absence of any dyestuif, which liquid medium is at an elevated temperature of at least 250 F. but below the softening point of the textile material, for a period of time sufficient to effect impregnation of the textile material with the heated organic liquid medium and to modify the fiber structure of the textile material by penetration of said organic liquid medium into said fiber structure but without otherwise affecting the fiber structure, removing the textile material from the heated organic liquid medium, and immediately thereafter contacting the textile material with relatively cool water, thereby substantially removing the adhering organic liquid medium from the textile material while leaving entrapped within the fiber structure thereof a small residual amount of said organic liquid medium.

5. A process as defined in claim 4 in which the organic liquid medium is at an elevated temperature of at least 350 F.

References Cited in-the file of this patent UNITED STATES PATENTS 2,461,612 Olpin et al Feb. 15, 1949 2,537,177 Woodrufi Jan. 8, 1951 2,663,612 Gibson Dec. 22, 1953 FOREIGN PATENTS 230,891 Switzerland Feb. 15, 1944 OTHER REFERENCES American Dyestutf Reporter, Nov. 13, 1950, page 790. 1 lgu Pang Bulletin CSB-D-35, Dacron, July 1954, pages

Patent Citations
Cited PatentFiling datePublication dateApplicantTitle
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Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US3022131 *Sep 3, 1957Feb 20, 1962Chem Fab Grunau VebProcess for increasing the colorability of polyester terephthalate fibers and the products obtained thereby
US3140957 *Feb 23, 1961Jul 14, 1964Kurashiki Rayon CoHeat treatment of fibers
US3154374 *Sep 12, 1961Oct 27, 1964Hoechst AgProcess for modifying the properties of shaped structures from highly polymeric polyesters
US3179484 *Aug 1, 1960Apr 20, 1965AcnaMethod for improving the dye-receptivity and dyeability of polypro-pylene
US3190718 *Apr 28, 1960Jun 22, 1965Celanese CorpProcess of heat treating a tow of polyester filaments while under tension to modify the properties thereof
US3222895 *Dec 1, 1961Dec 14, 1965Monsanto CoApparatus for treatment of napped fabric
US3245955 *Sep 12, 1961Apr 12, 1966Hoechst AgProcess for the manufacture of fibers and filaments of polyethylene terephthalate
US3251913 *Jun 1, 1961May 17, 1966Ici LtdProduction of a sheath-core polyester filament of enhanced dyeability
US3400187 *Feb 25, 1964Sep 3, 1968Fiber Industries IncMethod of treating polyester structures with polyalkylene glycol and a metal hyderoxide
US3427179 *Oct 23, 1965Feb 11, 1969Polymer CorpMethod of making a porous polyamide fabric
US3519462 *Mar 21, 1966Jul 7, 1970American Cyanamid CoMethod of impregnating polymethyl methacrylate
US3530214 *Feb 24, 1967Sep 22, 1970Bernard KlebanowMethod for treating textile materials to uniformly set their shape
US3617204 *Aug 27, 1968Nov 2, 1971Ici LtdHot glycol plasticizing removal of halogenated hydrocarbon solvent scouring liquor on polyester textiles
US3961882 *Jul 25, 1974Jun 8, 1976Bigelow-Sanford, Inc.Sculptured printing of nylon carpet
US4003880 *May 19, 1975Jan 18, 1977Monsanto CompanyFabric dye stripping, separation and recovery of polyester
US4003881 *Feb 24, 1975Jan 18, 1977Monsanto CompanyPolyester polymer recovery from dyed polyester fabrics
US4004878 *Oct 7, 1975Jan 25, 1977Chemische Werke Huls AktiengesellschaftProcess for the preparation of pilling-resistant fiber products from polyesters
US4115054 *Dec 15, 1976Sep 19, 1978Martin Processing, Inc.Process for the rapid, continuous and waterless dyeing and texturizing and heat-setting of textile and plastic materials
US4118187 *Dec 9, 1976Oct 3, 1978Monsanto CompanyFabric dye stripping, separation and recovery of polyester
US4550579 *Apr 13, 1984Nov 5, 1985Frank Clifford GApparatus for the dyeing of shaped articles
US4653295 *Aug 20, 1985Mar 31, 1987Frank Clifford GApparatus for the dyeing of shaped articles
US6221112Nov 2, 1998Apr 24, 2001Cp Films, Inc.Process for producing a colored polyester film
DE2716600A1 *Apr 14, 1977Jun 22, 1978Martin Processing Co IncVerfahren zum texturieren und thermofixieren von textilstoffen
Classifications
U.S. Classification442/164, 260/DIG.230, 8/922, 528/496, 8/611, 8/130.1, 427/353, 528/495
International ClassificationD06M13/52, D06M13/144, D06M13/53, D06P3/52, D06M15/53
Cooperative ClassificationD06M13/144, D06P3/52, D06M13/52, Y10S8/922, D06M13/53, Y10S260/23, D06M15/53
European ClassificationD06M13/53, D06M15/53, D06M13/144, D06P3/52, D06M13/52